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Chemicals & Equipment / Re: Supercritical CO2 extraction
« Last post by aniracetam on March 17, 2017, 01:39:01 PM »
parts list:

(all brass or stainless steel, except storage tank, and all rated for 3000psi, unless specified)

CO2 storage cylinder
1 10lb aluminum CO2 tank, rated @1800psi
1 CGA-320 cap and stem, with nylon disc (usually included)

3 Swagelok QF-4-S-4PF, quick connect stems, one connects to CGA-320 stem on storage tank, other two connect to needle valves on the sample cylinder

Sample Cylinder
1 Swagelok Whitey 1000CC sample cylinder, with two 1/4" FNPT ends, rated for 1800psi
2 Swagelok 1/4" MNPT needle valves, rated for 6000psi
400mesh SS screen, cut a small piece to stuff in needle valve on sample cylinder outlet

transfer hose assembly
2 Swagelok SS-QF4-B-4PF
2 Swagelok tees 1/4" FNPT
1 3000psi oil-filled pressure gauge, 1/4" MNPT
1 60" stainless steel braided, PTFE-lined hose with 1/4" MNPT ends
2 Swagelok needle valves, 1/4" MNPT, rated for 6000psi, one connects to tee connecting to sample cylinder, facing out..this will be for bleeding backpressure, to disconnect the transfer line
2  1/4" MNPT unions
1  1/4"  hex FNPT union

collection vessel, low pressure

3" x 12" sanitary stainless steel spool
1 3" triclover endcap
1 3" triclover endcap with two 1/4" FNPT inlets, or one with 1/2" (then also get a 1/2" to 1/4" FNPT bushing)
2 3" viton gaskets
2 3" triclover clamps
(connects to collection vessel inlet) 1 Swagelok QF-4-S-4PM
1 1/4" MNPT pressure relief valve, 140 psi

heating assembly
1 silicone heating pad, Omega part# SSHB-1224-720-120
1 PID temp controller, Mypin TA-4, with thermocouple
1 20A relay

note: remember to wrap PTFE tape around all brass-brass/brass-ss/ss-ss connections, 3 rounds. hand tighten connections as much as possible, mark across the connection with a permanent marker, then wrench tighten 1 1/4 turns (for 1/4" NPT connections, as specified by Swagelok).

the nice thing about this sort of setup is its modularity. one could swap out sample cylinders as needed. I also have a 1L Hoke cylinder rated for 5000psi operating pressure.
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Chemicals & Equipment / Re: Supercritical CO2 extraction
« Last post by aniracetam on March 17, 2017, 01:24:25 PM »
I assembled that extractor for >$700, not incl. the rolling island. it is an open loop system.
it is primarily Swagelok parts, 1/4" NPT. the sample cylinder is 1L, rated for 1800psi, but can easily handle 3000. the hoses are rated for 3000. needle valves are rated for 6000. The collection vessel is 316 sanitary stainless with a 150psi pressure relief valve. the silicone heating mat is rated for 750W. operating parameters for a typical run have been 1450-1600 psi @ 55C, temp monitored by thermocouple.

some notes about SC-CO2: it is primarily effective on nonpolar compounds, with m.w. up to 400. polar entrainers such as ethanol may be used to increase the effectiveness of pulling more polar compounds. It is advantageous to soxhlet for pulling nonpolar to somewhat polar compounds, as run times are typically 1-3 hrs, and it can extract thermolabile compounds to good effect. SC-CO2 has similar polarity to hexanes. all material should be dry as possible, as residual water freezes in the needle valves when they are opened, causing backpressure. this is caused by the joule-thompson effect.

I have used it to extract a variety of oils and extracts from star jasmine, lavender, pecans, 75 dried ghost peppers, cinnamon, cocoa, blueberries, vanilla, strawberries, apricots, guava, dill, lemon peel, mint, honeydew, coconut, banana, honeysuckle, and peach.
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Chemicals & Equipment / Re: Supercritical CO2 extraction
« Last post by hamsterbob on March 17, 2017, 10:48:06 AM »
I want a mr extractor!
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Chemicals & Equipment / Re: Supercritical CO2 extraction
« Last post by Halogen on March 17, 2017, 10:32:29 AM »
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Chemicals & Equipment / Re: Supercritical CO2 extraction
« Last post by aniracetam on March 17, 2017, 04:03:43 AM »
holy necroposting, batman..
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Publications / Re: Benzaldehyde Synthesis - Douchermann
« Last post by byko3y on March 17, 2017, 02:12:37 AM »
There's a lot of routes to convert alkyl halide to aldehyde. In fact, first step of kornblum oxidation is formation of alkyl halide form alcohol.
Hass-Bender reaction[1],  the Sommelet reaction[2],  the Krohnke reaction[3],  the Kornblum reaction[4],  the Masaki photooxidation[5],  and oxidations using NaOCl[6],  MnO2[7], KNO3[8], DMSO[9],  Pyridine N-Oxide in the presence of Ag2O[10], and transition metal complexes[11],  green oxidation of benzyl halides with V2O5-H2O2 [12] .
1. (a) Hass, H. B.; Bender, M. L. The reaction of benzyl halides with the sodium salt of 2-nitropropane: A general synthesis of substituted benzaldehydes. J. Am. Chem. Soc. 1949, 71, 1767–1769; (b) Klanderman, B. H. Aldehyde synthesis: A study of the preparation of 9,10-anthracene-dicarbox aldehyde and other aromatic dialdehydes. J. Org. Chem. 1966, 31, 2618–2620; (c) Klein, T. A.; Schkeryantz, M. S. Tandem Hass–Bender-Henry reaction for the synthesis of dimethylnitro alcohols from benzylic halides. Tetrahedron Lett. 2005, 46, 4535–4538.
2. Larock, R. C. Comprehensive Organic Transformation; John Wiley: New York, 1999; vol. 2.
3. Nishimura, T.; Onoue, T.; Ohe, K.; Uemura, S. Palladium(II)-catalyzed oxidation of alcohols to aldehydes and ketones by molecular oxygen. J. Org. Chem. 1999, 64, 6750–6754.
4. Kornblum, N.; Jones, W. J.; Anderson, G. J. A new and selective method of oxidation: The conversion of alkyl halides and alkyl tosylates to aldehydes. J. Am.. Chem. Soc.
1959, 81, 4113–4114.
5. Akichika, I.; Tomohiro, K.; Shinji, I.; Masaki, Y. Photooxidation of arylmethyl bromides with mesoporous silica FSM-16. Org. Lett. 2000, 16, 2455–2457.
6. Khurana, J. M.; Sahoo, P. K.; Titue, S. S. Ultrasound assisted oxidation of benzylic halides with sodium hypochlorite. Synth. Commun. 1990, 20, 1357–1361. 18 P.
7. (a) Goswami, S.; Jana, S.; Dey, S. A simple and convenient manganese dioxide oxidation of benzyl halides to aromatic aldehydes under neutral condition. ChemInform 2006, 36, 28–31; (b) Goswami, S.; Jana, S.; Dey, S.; Adak, A. K. A simple and convenient manganese dioxide oxidation of benzyl halides to aromatic aldehydes under neutral condition. Chem. Lett. 2005, 34(2), 194–195.
8. Liu, Q. F.; Lu, M.; Sun, F.; Li, J.; Zhao, Y. B. Oxidation of benzyl halides to aldehydes and ketones with potassium nitrate catalyzed by phase-transfer catalyst in aqueous media. Synth. Commun. 2008, 38, 4188–4197.
9. (a) Climent, M. S.; Marinas, J. M.; Sinisterra, J. V. Ba(OH)2 catalyst in organic reactions, XIII. Oxidation of benzyl halides to benzaldehydes. React. Kinet. Catal. Lett. 1987, 34(1), 201–206; (b) Bratulescu, G. Synthesis of aromatic aldehydes by a fast method involving Kornblum’s reaction. Synth. Commun. 2008, 38, 2748–2752; (c) Kshirsagar, S. W.; Patil, N. R.; Samant, S. D. Mg–Al hydrotalcites as the first heterogeneous basic catalysts for the Kornblum oxidation of benzyl halides to benzaldehydes using DMSO. Tetrahedron Lett. 2008, 49, 1160–1162.
10. Chen, D. X.; HO, C. M.; Wu, Q. Y. R.; Wu, P. R.; Wang, F. M.; Wu, W. M. Convenient oxidation of benzylic and allylic halides to aldehydes and ketones. Tetrahedron Lett. 2008, 49, 4147–4148.
11. (a) Griffith, W. P.; Jolliffe, J. M.; Ley, S. V.; Williams, D. J. A new ruthenium(VI) oxidant: Preparation, X-ray crystal structure, and properties of (Ph 4 P)[RuO 2 (OAc)Cl 2 ]. J. Chem. Soc., Chem. Commun. 1990, 18, 1219–1221; (b) Peyman, S.; Irai, M-B. Tetrakis (pyridine)silver(II)peroxodisulfate, [Ag(py) 4 ]S 2 O 8 , a reagent for the oxidative transformations. Bull. Chem. Soc. Jpn. 1992, 65, 2878–2880; (c) Bressan, M.; Forti, L. Ruthenium-catalyzed oxidation of alkylaromatics by monopersulfate with preferential oxidative fission of the benzene ring. J. Mol. Catal. 1993, 84, 51–58.
12. Li, C. B.; Zheng, P. W.; Li, J.; Zhang, H., Cui, Y.; Shao, Q. Y.; Ji, X. J.; Zhang, J.; Zhao, P. Y.; Xu, Y. L. The dual roles of oxo diper oxo-vanadate both as a nucleophile and an oxidant in the green oxidation of benzyl alcohols or benzyl halides to aldehydes and ketones. Angew. Chem. Int. Ed. 2003, 42, 5063–5066.
Have fun.
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Publications / Re: Benzaldehyde Synthesis - Douchermann
« Last post by Halogen on March 17, 2017, 12:20:34 AM »
what about benzyl bromide as a sommelet reaction precursor? i know it's theoreticaly possible, but what about practice? ever tried it instead of benzyl chloride?
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Publications / Re: ketones and stuff
« Last post by carl_nnabis on March 16, 2017, 11:00:17 PM »
Well I wouldn´t call that stalker who´s putting random chemical notes in my life a friend, but yeah, there was really a little bit of information about this attempt(incomplete though).

It says 11mmol of Isonitrosoketone and 67mmol of Na were used, an amine-like odour was noticed during the reaction, but no mention of product obtained if any at all(I don´t think so).
I assume, since the reduction of this nitrosoketone is described as hard to achieve(compared to other oximes), that he failed.

A literature source describing the complete reduction, using catalytic hydrogenation, mentions the presence of HCl as being vital for success.
Lead me to theorise that the formation of a pyrazine, a dimer is probably a competing reaction in the basic milieu of a Na/EtOH reduction, whereas the cathinone formed as intermediate dimerises to said pyrazine.

This is also the reason why I assume an Al/Hg reduction(acidic, with AcOH) is a better choice.
Probably even better would be, to do it in two steps, reducing the carbonyl to an alcohol first with borohydride.
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Publications / Re: ketones and stuff
« Last post by bsmathers on March 15, 2017, 11:39:38 PM »
Did your Bulgarian friend also happen to leave a writeup of the attempted sodium reduction?  ;D

I have a hard time believing that an amalgam reduction would work better than an alkali metal one, considering the problem in my mind is incomplete reduction. Then again, I have been wrong before...

I wonder if lithium would be a worthwhile thing to try?
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Publications / Re: ketones and stuff
« Last post by carl_nnabis on March 15, 2017, 09:18:11 PM »
Hey! Here´s some more, maybe of interest?

I was going for a walk, stepped into some gum and when I tried to remove it, I discovered a note sticking to it, with the following information written on it. As usual with "my" stalker, it was written in bulgarian, but the translation was straightforward.

It says:
Quote
Part III: Propiophenones related aminoketones, third part.

Since a wide variety of substited cathinone derivates can be had with ease using the "NBS-method", it was decided to dive deeper into the related aminoketones, this time with a little more structural unusual analogues.
Instead of being restricted only to aromatic substitions on propiophenone, other interesting features were tried out.

Like longer side-chains or another aromatic heterocycle instead of benzene.
A very promising aromatic substituent on plain propiophenone was used as well.
Some of the resulting substances turned out to be quite euphoric and very enjoyable, worth the effort, and some were not.
Chemical-wise, nothing novel is described in this part which isn´t already present in the former ones.
Also, the ketones were all acquired from big brands and not china, good quality and thus expensive(=the price of being lazy). So nothing new about their preparation too, sorry.   

The 3-fluorinated cathinones are worth to be mentioned especially, as they are potent dopamine releasers, and a good amount of serotonine too, but lacks considerable noradrenergic effects in comparison.
That makes for some fine euphoric substances, but with much less strong physical stimulation, making the overall experience very pleasant.
So far, the 3-fluoro substitution lead to some of the most enjoyable cathinones tried.
 
The cathinone analogues of thiophene or the "thiothinones", are sadly nowhere as good, being less than half as potent than their respective phenyl-counterparts.
The starting ketone smells a lot nicer than propiophenones, creamy with a hint of caramel and not unpleasant.
Some heterocyclic analogues of cathinones seemed cool and the choice between the thiophene-, indane-, or naphthyl-derivative had to be made.
Looking back, the naphthyl- would have been a much more rewarding choice.
The heterocyclic cathinones sparked some scientific interest, without having special pharmacological properties(By the way for anyone interested where the sulfur goes, it gets excreted, renal I think, as thiophen-2-yl carboxylic acid).

And finally, hexanophenone was used to prepare the methyl- and ethylamino derivatives, who turned out to be quite potent compared with their propiophenones, euphoric and stimulating.
It is worth to mention, that the butyl-analogue of methcathinone is less potent than the latter, but the pentyl- and longer chain analogues are becoming more potent with increased length.
The most interesting feature of the N-ethyl derivative, is its threefold potency compared to its N-Methyl analogue, because of shifted electronegativity due to longer alpha-alkyl- and N-alkyl-chains.
The ethylamino derivative is said to have local anaesthetic effects, and very weakly it could be felt when a few mg´s were applied on tip of the tongue.
Those are called, similar to ephedrone, "hexedrone" and "ethyl-hexedrone".
Their precursor smelled propiophenone-esque, but heavier, better and "greener", also a little hint of wax.


- 2-(pyrrolidino)-1-(2-thienyl)-1-propanone/alpha-Pyrrolidinopropionylthiophene(alpha-PPT) (7.A.)

Experimental:
Analogous to 5.A., the following amounts were used:
-2g of 2-propionylthiophene(14,28mmol) was dissolved in about ~3-4ml of MeCN in a flask, to which
-2,84g of N-Bromosuccinimide(16mmmol) were added and a further quantity of
-300mg p-Toluenesulfonic acid(1,6mmol).
The resulting mixture was treated as in 5.A., heated for ~2,5 hours.
The cooled down mixture was worked up as in 5.A., but product instead taken up in 25ml MTBE, organics brine- and soda-washed, then dried(Na2SO4).

The bromoketone in MTBE was, under stirring, placed in a 100ml erlenmeyer sitting in an ice-salt bath, then
-2,2g/2,54ml pyrrolidine (31,41mmol), dissolved in a 1-2 ml of MTBE, were added in one portion, causing the mixture to turn yellow, half an hour later a small oily layer was seen at the bottom, which was expected but not observed with DCM as in 5.A.
Half an hour later, the cooling bath is removed and the reaction mixture continues to be stirred at room-temperature for the next 24 hours. Then 20ml of dH2O were added, the organics separated and the aq. portion extracted once with 15ml MTBE, the collected organics were washed with brine(20ml) once, then dried and extracted into 5% HCl two times.
Aqueous extract was evaporated, the solids taken up with 25ml DCM and filtered, volume reduced to a few ml and 40ml acetone added and allowed to cool a litte.
Then put in the freezer(-18°C) for a few hours, filtered, washed with two portions cold acetone, and air-dried.
It gave a final yield of 422mg HCl-salt(1,7mmol, just 12% of theory), having a melting point of 198°C

Bioassay:
When it was tried out, dosages ranging from 20-90mg were used, and the overall experience is qualitative not very distinguishable from alpha-Pyrrolidinopropiophenone. It has similar effects in every aspect to the latter substance, just seems to be a bit less potent on a subjective level than it´s "cousin".
Which was expected, but with this compound negligible(someone got the pharmacological datas for this one?).
A nice and talkative, not overly physical stimulating substance, giving a good euphoric mood.
Good for talkative socialising, but not much for doing intellectual tasks though.
Total duration seems to be around 3-5hours, with its effects reaching the peak after 5-10 minutes and staying there around an hour, at which point redosing will sustain the effects.


- 2-(ethylamino)-1-(2-thienyl)-1-propanone/"Ethiothinone" (7.B.)

Experimental:
This one, made using the same process as 0.A. and 1.A., used the following reagents:
-3g of 2-propionylthiophene(21,41mmol), dissolved in about ~5ml MeCN, then
-4,26g/24mmol of N-Bromosuccinimide were added, followed by
-456mg of p-Toluenesulfonic acid (2,4mmol, the monohydrate, thanks Kykeon ;)), after which the reaction mixture was heated gently to 60-70°C, while heavily stirred, during which time all the solids go into solution.
The solution was further heated under stirring at this temperature, until a TLC sample taken at 2,5 hours indicated the starting material had reacted.
The reaction was let to cool down, and after reaching room temperature, 15ml DCM and an equal amount of dH2O was added, allowed to settle and the DCM separated.
This layer was washed with ~25ml of 5% Na2CO3 solution, then another two times using saturated brine solution.
The DCM containing the bromoketone was now dried over Na2SO4, then filtered and again put into a flask.

This was set up in the ice-salt bath, stirred heavily, and portion-wises a solution weighing
-3,44g of an 70% aqueous EtNH2(133mmol) solution was added to the mixture over the course of five minutes.
The whole reaction mixture was allowed to react, stirred heavily, over night while sitting in an ice-salt bath.
The next day TLC showed no more bromoketone, so to the reaction mixture an equal amount of dH2O was added under gentle shaking, and after it settled the DCM was drawn of, washed(1x dH2O, 1xbrine), then dried(Na2SO4).
To the organic phase, around 10ml dH2O were added and drop-wise diluted HCl too, until pH nearly neutral, then another
acidic pull was done and both combined for evaporation.
The residual solids were dissolved in boiling DCM(around 30ml), filtered from insolubles after cooling down a little, and reduced in volume to a few milliliters. To this, hot acetone is added and the whole mixture put aside for few hours at RT, then overnight around like ~ -18°C.
The crystals are broken up, filtered and rinsed two times with cold acetone, then air-dried, to give a "stellar" yield of 212mg HCl salt(0,96mmol, like 4,5% of the theory).

No bioassay was done with this stuff, probably isn´t even enough yield to quantify the effects properly.
But it can be concluded that it will be at most half the potency of its phenyl-counterpart, more likely only a third or even less.
Still not sure about every source(s) of failure(s) regarding the extremely low yield. Mother liquor also did not yield any substantial further amount, only dirty stuff unworthy of wasting solvent for.


- 3-Fluoro-N-Ethylcathinone (8.A.)

Experimental:
Analogous to 0.A and 1.A., the reaction was carried out with the following amounts:
-3g of 3-Fluoropropiophenone(19,74mmol), dissolved in about ~5ml of MeCN, to which
-3,94g N-Bromosuccinimide(22,2mmol) were added, followed by
-380mg of p-Toluenesulfonic acid(2,2mmol),
and the resulting mixture was treated in the same manner to obtain a solution of the bromoketone in DCM, which was under stirring placed in an ice-salt bath.

To the cooled mixture, 
-3,22g Ethylamine as 70% solution (50mmol) were added and stirring was continued in the cooling bath, for around ~10 hours overnight.
It was worked up exactly as in 1.A., sitting at -18°C for a night to crystallise out, and when filtered and dried, the final yield was 1,21g of the HCl salt(5,2mmol, or 26% of the theory).
A bit disappointing, but being in the form of small attractive white needles it was ok. Recrystallisation with DCM/acetone improved their appearance further.

Bioassay:
This one has very pleasant effects, but a short duration, best description would be an afterwork stimulant, total effect
of 2-3 hours, peak about 60 minutes, and euphoria can be felt very fast. It is both good for doing work or having a good
time with someone else.
Subjective effects indicate a good balanced releaser of all three importants neurotransmitters, making it pleasant and thus abusable. Dosages used ranged from 15-60mg.
Reinforcing too, since it´s a fun experience.


- 3-Fluoro-alpha-Pyrrolidinopropiophenone/3F alpha-PPP(3F-alpha-PPP) (8.B.)

Experimental:
The bromoketone was prepared analogous to 5.A., using the following amounts:
-2g 3-Fluoropropiophenone(13,16mmol), dissolved in 4ml MeCN,
-2,63g N-Bromosuccinimide(14,8mmol), and finally
-254mg p-Toluenesulfonic acid(1,4mmol),
heated for 2,5hours, worked up similar to 5.A. but instead extracted into 25ml MTBE.

The washed and dried organics were, under cooling, reacted with
-2,06g/2,37ml of Pyrrolidine(29mmol), added at once under stirring, and after being cooled for 1 hour, removed from the
bath and stirred at RT for a further ~24 hours. Equal amount of dH2O was added, layers separated and further work-up was done as in 7.A., but instead of extracting the MTBE containing the product freebase using aqueous HCl, some dry IPA containing HCl was added till nothing precipitated anymore.
These filtered solids were washed with cold acetone(2x20ml), air-dried and recrystallised using DCM and acetone, to obtain a final yield of 1650mg HCl(6,4mmol, corresponding to 48% of theory), which was melting at around 208-212°C.

Bioassay:
This one was assayed in dosages ranging from 20-50mg, intranasally, and was found to be a very enjoyable albeit very little physical stimulating, normally associated with noradrenergic effects, but lots of euphoria and social talkativeness instead which indicates it affect mostly dopamine. Some yawning was also noted at the beginning, which hints to serotonergic activity too. Peak effect, is reached after 10-15 minutes via this route of application, and stays there for 60-120 minutes, then begin to weaken until after 5 hours it is gone mostly.
Total duration being 3-5 hours estimated.
Quite reinforcing due to the euphoria, but less suited for boring tasks, it is better to be used in company of someone.
Acts as potent aphrodisiac too.


- 2-Bromohexanophenone (9.A.)

Experimental:
Similar to 0.A., a solution of
-5g Hexanophenone(28,4mmol),
-5,7g N-Bromosuccinimide(32mmol), and
-550mg p-Toluenesulfonic acid(3,2mmol) in ~5ml MeCN was prepared,
and heated at 60-70°C under strong stirring for about 2 hours, after which the starting ketone had reacted.
After the extraction using DCM, washing and drying of solvents, the DCM solution(~30ml) was divided into a larger, around 2/3(for 9.B.), and a smaller portion, 1/3 of total volume(for 9.C.).

- N-Ethylaminohexanophenone ("N-Ethylhexedrone") (9.B.)

Experimental:
Two third of the bromoketone solution(containing ~19mmol bromoketone/~20ml DCM) were reacted with
-3g of a 70% EtNH2 solution(47mmol) in an ice-salt bath, stirred strongly, for about 12 hours(overnight).
To the resulting mixture was added, after that time-periood, about ~25ml of 2H2O, layers separated, washed with brine,
dried(Na2SO4) and titrated, aq. portion evaporated, residue extracted with DCM and filtered, volume reduced and two times as much acetone as original volume added, then left to cool.
When filtered and washed with few times using cold acetone, total yield was 2055mg HCl-Salt(8,03mmol), which corresponds
to 42% of the theory, with a mp of 182-184°C, forming very nice needles when recrystallised from H2O/IPA over a longer time period.

Bioassay:
This substance has very similarly pleasant effects to ethylcathinone, at the time one of the most favored cathinones.
Euphoric stimulant with aphrodising properties, very good to complete tasks and monotonic work too, like typing, drawing
or calculating things. This one is used in dosages from 10 up to 60mg, and with its total duration of up to 5 hours a
slightly longer duration than other cathinone-like substances. Peak effects are felt 1-2 hours, depending on the dosage.
Also, it is very slightly locally anaesthesic, when it touches mucous membranes, mostly can be felt at the tip of
tongue. 
The aminoalkane is probably a promising thing to make.

- N-Methylaminohexanophenone ("Hexedrone") (9.C.)

Experimental:
One third of the DCM-bromoketone solution(~9,5mmol/~10ml DCM) was filled up to around 25ml DCM in total, and then reacted with an ice-cold solution made of
-1,55g MeNH2-HCl(23mmol) in 2-3ml dH2O, and
-0,91g of NaOH(23mmol) in 2ml dH2O, and then reacted in the ice-salt bath for around a half day.
The work-up was done as with 9.B., and gave after air-drying just 405mg of the HCl salt(1,67mmol, corresponding to sad 7,5% of theory). When recrystallised from 70% IPA, it was forming tiny sparkling needles.

This compound was not yet bio-assayed, given the much lower potency than it´s N-ethyl derivative, it seemed not that much appealing at all, but will be assayed someday, if solely for the purpose of quantifying the difference to the former substance.


- Conclusion:
The NBS-method seems to be so widely applicable for the synthesis of aminoketones, it´s boundaries are yet to be touched with the tried substrate ketones.
And a lot of fun too, more people should give it a try!

It is worth to mention, that every brominated ketone had lachrymatoric properties, more or less but not one has been without this property.

In a possible next part, some novel stuff will be included again, maybe a mannich reaction on a ketone, and something like FC-acylation of an aromatic heterocycle, with an acid anhydride instead of acid halide maybe.
Also planned, to reductively aminating acetylbenzoyl with ethanolamine or similar hydroxylalkylamine.

Hope this stuff is of use for anyone, and not just some boring cathinone-stuff!

The attachments contain the reference used for preparation of pyrrolidinoketones, and a bad drawing of the reaction scheme as well.
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