Author Topic: Short Question Thread 2.0  (Read 5707 times)

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #180 on: September 10, 2012, 05:31:24 PM »
lugh, i apologise for me asking such things I knew already about, but this community faciliates a tendency in me being lazy!  :-X
Without I would have probably already have made some Et2O on my own, and a good amount was also made now, costs were less then a 20th of bought one. I also knew already about the properties of DIPE regarding peroxide formation  ::)
Just wanted to know about the schlenk equilibrium but figured it already out even if its not of use now anyway.

For DCM, i was talking about acidic solutions and its not really an emulsion im talking about there?

Oerlikon, your diacetylmorphine is nearly insoluble in anything beside methanol and aromatic hydrocarbons, so should be easy to figure out i guess?
« Last Edit: September 10, 2012, 05:33:10 PM by carl_nnabis »
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embezzler

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Re: Short Question Thread 2.0
« Reply #181 on: September 16, 2012, 10:59:49 AM »
Apologies for the laziness but does anyone have a nice staining protocol for c. purpurea sclerotia. I want to look a little closer at this under 100x. Thanks in advance.
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lugh

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Re: Short Question Thread 2.0
« Reply #182 on: September 16, 2012, 06:42:39 PM »
Color tests for indoles from Smith's Psychedelic Chemistry:

Identification of Indoles
Keller Test

Add a little of the powdered substance (about 0.2 mg to 1 ml glacial acetic acid containing 0.5% FeCl3, layer underneath with 1 ml concentrated sulfuric acid and shake. The color varies with the indole, being olive green for psilocin and red-violet for psilocybin.
Van Urk Test

Prepare Van Urk reagent by adding 0.5 g p-dimethylaminobenzaldehyde, 100 ml water, 100 ml concentrated sulfuric acid. Dissolve 1 mg substance in 1 ml ethanol and mix with 2 ml Van Urk reagent and illuminate for 10 minutes with an ultraviolet lamp (black light). Psilocin gives a blue-grey, psilocybin a red-brown color. Colors produced in these two tests by many indole derivatives are given in HCA 42,2073(1959).
Quick, Easy, On-the-Spot Test JPS 56,1526(1967)

Saturate strips of filter paper with 2% p-dimethylaminobenzaldehyde in 45% ethanol; air dry and store in tightly stoppered amber bottles (or keep in stoppered container in dark) which will keep them useful for several months. Put a little of the suspect substance in a few drops of ethanol (gin may do, but do a control), wet a filter paper strip in this and allow to dry. Put one drop concentrated HCl on the dried paper (don't let it touch anything). Alternatively, the powder can be placed directly on the strip and the HCl dropped on it. A violet red or violet blue spot indicates indole derivatives such as LSD. With DMT or psilocybin the color is redder. The color must be observed soon after adding the HCl since it rapidly changes.


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DopeBee

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Re: Short Question Thread 2.0
« Reply #183 on: September 18, 2012, 02:41:29 PM »
Are the following chemicals all the same?

N-phenethyl-4-piperidinone
N-phenethyl-4-piperidone
1-phenethyl-4-piperidone
1-(2-Phenylethyl)-4-piperidone
N-(2-Phenethyl)-4-Piperidone
« Last Edit: September 18, 2012, 02:49:01 PM by DopeBee »

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #184 on: September 18, 2012, 03:01:37 PM »
yes because it is 1-(c6h5 so phenyl or short phen and 1- because its on 1 which is N in most cases if present, for example look at indole, then ch2-ch3 or ethyl which, because it is the last substituent in the naming of this group precisely and has then phenylgroup on its second carbon, so there a 2-.

addition: wtf is going on with the 4-? it is because it is named for for the 4- position of piperidon, because if oxygen is present too than thats primary in counting, like in phenmetrazin or such.

another name maybe could be n-(4-piperidinone)-2-phenylethylamine?
« Last Edit: September 19, 2012, 04:14:57 PM by carl_nnabis »
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Goldmember

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Re: Short Question Thread 2.0
« Reply #185 on: September 19, 2012, 05:03:03 AM »
Stupid question maybe, but Ive found numerous descriptions.

What colour is anhydrous reagent grade  Ferric Chloride, quality enough to use as Friedel-Craft catalyst?

  Ive come across some very dark brown chloride,with flecks of caramel, but it isnt exactly what Id call green/black,(purple depending on the light) as per most descriptions Ive seen and its in the form of fine powder as opposed to crystalline.
This stuff does fume somewhat when open to air. Ive attempted to further dehydrate a sample in a stream of dry HCl with no noticable colour change.

Anyone with real word experience?

lugh

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Re: Short Question Thread 2.0
« Reply #186 on: September 19, 2012, 12:25:14 PM »
Quote
Stupid question maybe, but Ive found numerous descriptions.

What colour is anhydrous reagent grade  Ferric Chloride, quality enough to use as Friedel-Craft catalyst?

  Ive come across some very dark brown chloride,with flecks of caramel, but it isnt exactly what Id call green/black,(purple depending on the light) as per most descriptions Ive seen and its in the form of fine powder as opposed to crystalline.
This stuff does fume somewhat when open to air. Ive attempted to further dehydrate a sample in a stream of dry HCl with no noticable colour change.

Anyone with real word experience?

It's a dark brown powder, and the preparation has been discussed in:

https://the-collective.ws/forum/index.php?topic=11013

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EMTWC

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Re: Short Question Thread 2.0
« Reply #187 on: September 19, 2012, 03:34:04 PM »
finally achieved some relative success after much bone headedness. Rule number one, DON'T drink the 40>>>more for a longer, more humorous post

https://www.erowid.org/archive/rhodium/clandestine/methylamine/index.html

BUT>>>final result is like flos grits. Assume not enough water was boiled off. Which leads to>>>

best way to dry it out????
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lugh

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Re: Short Question Thread 2.0
« Reply #188 on: September 19, 2012, 05:22:30 PM »
Quote
BUT>>>final result is like flos grits. Assume not enough water was boiled off. Which leads to>>>

best way to dry it out????

Your question is almost incomprehensible, and it's clear your understanding of this language is minimal  ::) The best way to dry it isn't mentioned due to the expense involved  ;) The attached documents from the Organic Syntheses website  and Wikipedia explain the relevant facts very well :-X  You need to reread the threads you're quoting from many more times, and start looking for more sources of information online  :P  The information you seek is available in other languages :)  Bright Star has a PhD from a prestigious university, and his method to mdma isn't exactly crude as it has worked for thousands of members  :-X  The end results from the effort applied  8)
« Last Edit: September 20, 2012, 04:42:29 AM by lugh »
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EMTWC

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Re: Short Question Thread 2.0
« Reply #189 on: September 19, 2012, 08:59:12 PM »
Quote
BUT>>>final result is like flos grits. Assume not enough water was boiled off. Which leads to>>>

best way to dry it out????

Your question is almost incomprehensible  ::)

The end results from the effort applied  8)

admitted that comprehension isn't a strong suit. Need to get the hands dirty to learn anything.
will review the attachment, thank you kind sir.
roll some bones and catch a fire

EMTWC

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Re: Short Question Thread 2.0
« Reply #190 on: September 20, 2012, 01:12:51 AM »
2nd batch turned out much less "wet"...let it boil longer. After that, had a chance to read lugh's attachment, interesting indeed. I think the key words left out of Rhodi's photo essay were "until crystals begin to form on the surface".  Although, now looking back, they can be seen in the picture.


So it would appear that Brightstar method=crude, the rhodi method pretty darn close, and the winner would be organ syth vol 1 pg 347>>>

only trick is how to centrifuge????

3rd batch brewing. will boil til crystals form on top.

How essential are the the chloroform washes?

also...brightstar says 4 hours, rhodi says 3-4, luhg's ref says 5-6, jon says 6>>>sounds like a choose your own adventure>>>

« Last Edit: September 20, 2012, 03:27:49 AM by EMTWC »
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Tsathoggua

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Re: Short Question Thread 2.0
« Reply #191 on: September 24, 2012, 09:06:04 AM »
What is the approximate time course required to go from aldehyde->aldoxime->hoffmann ?
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carl_nnabis

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Re: Short Question Thread 2.0
« Reply #192 on: September 24, 2012, 09:40:36 AM »
Consider you have to do the beckmann rearrangement before the hofmann rearrangement can take place.
About the time, i think it can be done in less than 2 two days if every reagent is available, but i dont know for sure.
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Tsjanga

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Re: Short Question Thread 2.0
« Reply #193 on: September 24, 2012, 11:45:27 AM »
Yeah you can do it within 2 days if you want, first step 4/6 hours, second step 6/7 hours and hofmann about 2 hours in total.

Now a question from me:
How much solvent do you need to get your freebase out of the hofmann rxn?
Is there a simple ratio when you use IPA?

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #194 on: September 24, 2012, 12:04:35 PM »
as a rule of thumb, use 2 times a tenth of mother liquor volume and the third time one part on twenty suffices. Just let every layer sit long enough, and avoid an emulsion.
Also, dont use IPA, better suited would be hexane or toluene/xylene, IPA has to be salted out afterwards otherwise its completely miscible with water.
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Tsjanga

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Re: Short Question Thread 2.0
« Reply #195 on: September 24, 2012, 02:06:13 PM »
as a rule of thumb, use 2 times a tenth of mother liquor volume and the third time one part on twenty suffices. Just let every layer sit long enough, and avoid an emulsion.
Also, dont use IPA, better suited would be hexane or toluene/xylene, IPA has to be salted out afterwards otherwise its completely miscible with water.

Thanks!
So 1:10 xylene:freebase and then 1:20 xylene:freebase would be fine am I right?
With xylene the dog wouldn't get trouble gassing the hell out of it with HCL right?

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #196 on: September 24, 2012, 04:29:27 PM »
Well, tell your dog he should add some suited drying agent ;)
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Tsjanga

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Re: Short Question Thread 2.0
« Reply #197 on: September 24, 2012, 05:02:19 PM »
Well, tell your dog he should add some suited drying agent ;)

Yeah he already told me that he would do it!
Can you tell me how much he would need to get 1 liter of xylene free of H2O, or is there some way to see it is free of H2O?

lugh

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Re: Short Question Thread 2.0
« Reply #198 on: September 24, 2012, 05:52:39 PM »
Well, tell your dog he should add some suited drying agent ;)

Yeah he already told me that he would do it!
Can you tell me how much he would need to get 1 liter of xylene free of H2O, or is there some way to see it is free of H2O?

Xylene and water form a lower boiling point azeotrope:

h**p://en.wikipedia.org/wiki/Azeotrope

h**p://en.wikipedia.org/wiki/Azeotropic_distillation

You need to start learning about practical organic chemistry from textbooks instead of posting such questions:

http://library.sciencemadness.org/library/books/vogel_practical_ochem_3.pdf

http://library.sciencemadness.org/library/books/the_practical_methods_of_organic_chemistry.pdf

http://library.sciencemadness.org/library/books/practical_organic_chemistry.pdf

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Electro´S

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Re: Short Question Thread 2.0
« Reply #199 on: September 25, 2012, 12:56:21 AM »

How essential are the the chloroform washes?


How pure you need your product?

Jon is the best. boil under vaccum in Salt/water bath (106ºC) until your product smoke inside the flask than turn off all and choose your way to recover it.  In this way you can avoid chloroform but If you heat more than 106º chloroform is required.