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Author Topic: Bet you can't post awesome OTC reagents/synthesis I've never seen before  (Read 387 times)

Enkidu

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Bet you can't post awesome OTC reagents/synthesis I've never seen before
« on: October 04, 2011, 05:48:13 PM »
I'm using OTC loosely.

Try me.

For each solid attempt, I'll post something in return.

Balkan Bonehead

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #1 on: October 04, 2011, 09:22:02 PM »
Aspartic acid + TCCA ---oxidative decarboxylation---> cyanoacetic acid ---hydrolysis---> malonic acid.

akcom

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #2 on: October 04, 2011, 10:23:31 PM »
Thank god we can now filter the fucking catalyst out of our reaction now.

Pd(0)/C catalyzed efficient Wacker oxidation of functionalized terminal olefins
Tetrahedron Letters
Vol 50 (2009) pp 2893–2894
Mukund G. Kulkarni *, Sharanappa M. Bagale, Mahadev P. Shinde, Dnyaneshwar D. Gaikwad, Ajit S. Borhade, Attrimuni P. Dhondge, Sanjay W. Chavhan, Yunnus B. Shaikh, Vijay B. Ningdale

Although I'm a bit worried if they really think Pd(0) is whats catalyzing this reaction

Balkan Bonehead

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #3 on: October 05, 2011, 12:24:31 AM »
Quote from: java on October 04, 2011, 10:44:50 PM
Toluene + ethylacetate------>>*KOEt------>>>>Phenylacetone

* KCO2 + EtOH----->>>  KOEt  + KCO2  or  KOH +EtOH----->>  KOEt + EtOH


Ref: ETHYL INDOLE-2-CARBOXYLATE

      Transformations of electrophilic reagents in a diethyl phosphite--potassium carbonate--ethanol system

       Advanced_Techniques_of_Clandestine_Psychedelic__amp__Amphetamine_Manufacture -Page 50-56

That won't work out, bro. The aromatic nitro group is required to elicit an electron-withdrawing effect and facilitate the condensation.


....it just looked like an easy Rx but know very little about it.....so i deleted it .........java
« Last Edit: October 05, 2011, 02:03:27 AM by java »

Wizard X

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #4 on: October 05, 2011, 01:30:32 AM »
Advanced_Techniques_of_Clandestine_Psychedelic__amp__Amphetamine_Manufacture -Page 50-56 at e-book Library are broken.
http://127.0.0.1/talk/index.php/topic,794.msg9475.html#msg9475
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Enkidu

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #5 on: October 05, 2011, 03:36:06 AM »
These two are, IMO, fairly well known, but lets start small. They haven't been posted here at TV yet.

The following paper discusses the oxidation of ethers to esters (THF-->GBL). It also notes the preparation of benzaldehyde from benzyl alcohol using TCCA.

Direct conversion of ethers to esters by trichloroisocyanuric acid
Juenge and Beal
Tetrahedron Letters 1968 55:5819-5820

The next is the Mg formylation of 4-methoxyphenol.

US2003199714A1 Process for preparing 2,5-dimethoxy benzaldehyde mg.paraformaldehyde.triethylamine formylation.pdf
« Last Edit: October 05, 2011, 03:37:52 AM by Enkidu »

nk40ouvm

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #6 on: October 05, 2011, 08:38:23 AM »
Grab the book Small-scale synthesis of laboratory reagents with reaction modeling from your favorite book warez site. It's written by Leonid Lerner, a.k.a. "len" "len1" len2" on Sciencemadness. As a human being he's a bit of a dick, and several of his syntheses are based on information that he borrowed without acknowledgment from other members' Sciencemadness posts, but he's a good hands-on chemist and has refined all of these syntheses to a high degree. They are designed for a small academic chemistry department, but most start with common materials and can be performed with less than $1000 worth of equipment, so they are OTC (advanced-OTC) by my reckoning.

You shouldn't ignore any of what he writes, but here are some highlights:

Phosphorus oxychloride from calcium triphosphate, charcoal, and chlorine*
Lithium chloride to lithium metal
Lithium metal to lithium hydride
Aluminum metal to aluminum bromide
Aluminum bromide + lithium hydride to lithium aluminum hydride
Sodium bisulfate to oleum
Sulfur to sulfur dichloride
Sulfur dichloride + oleum to thionyl chloride

*This one's based on a patent that you have likely seen posted on forums before, but he actually took the time to develop it on a lab scale, write it up, and take pictures.

Enkidu

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #7 on: October 05, 2011, 09:08:05 AM »
^ Yeah, I have had my hands on a hard copy of that one ;) Nice suggestion.

Toluenesulfonic acid can be subbed for the methanesulfonic acid.

Mona Hosseini Sarvari, Hashem Sharghi
Simple and Improved Procedure for the Regioselective Acylation of Aromatic Ethers with Carboxylic Acids on the Surface of Graphite in the Presence of Methanesulfonic Acid
Synthesis, 2004, 2165-2168. DOI: 10.1055/s-2004-831162

no1uno

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #8 on: October 05, 2011, 01:21:02 PM »
On that note, has anyone got a scanned copy of that book? It grabbed my attention quite a while back when I found the phosphoryl chloride synthesis and workup - it looked like SM type apparatus which caught my eye (actually looked like Stefan's/GC's gear, some of it). I have no drama with Len/Len1, his bitch fights with Sauron were legendary.
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salat

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #9 on: October 05, 2011, 04:30:26 PM »
it's at:

http://library.nu/search?q=small-scale

about 1/2 page down in the list.
Salat

reDEEMed

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #10 on: October 05, 2011, 07:42:50 PM »
It's also only $120 on amazon.
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Sydenhams chorea

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #11 on: October 19, 2011, 09:01:09 PM »
2,5-dimethoxytetrahydrofuran as chief product in good yield from the anodic oxidation (no diaphragm) of malic acid in MeOH/NaOMe.  Downside = Pt electrodes but I bet graphite can substitute. Not at home right now so I'll give the ref later.

OTC succinic dialdehyde... How about them apples?
It is perhaps the narcotic. Hyoscine affects certain people very oddly. One cannot be sure. Sometimes, these cases take strange forms. The victim becomes in a sense, 'mediumistic', a vehicle for all the intangible forces in operation around her.

Sydenhams chorea

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #12 on: October 19, 2011, 09:11:57 PM »
Also from memory:

sugar + acid + heat --> levulinic acid, ester when done in alcoholic environment

reduction gives  gamma-valerolactone (weaker version of GHB) but perhaps more interestingly: Fisher indole synthesis with phenylhydrazine gives 2-methylindoleacetic acid.
It is perhaps the narcotic. Hyoscine affects certain people very oddly. One cannot be sure. Sometimes, these cases take strange forms. The victim becomes in a sense, 'mediumistic', a vehicle for all the intangible forces in operation around her.

Sydenhams chorea

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #13 on: November 05, 2011, 11:28:17 AM »


http://www.electrochem.org/dl/ma/197/pdfs/1059.pdf

MECHANISTIC ASPECTS CONCERNING ANODIC OXIDATION OF CARBOXYLIC ACIDS

Quote
Similar behaviour has been found in
the case of glutaric acid oxidation [3], even if
in this case g-butirolactone formation takes
place with a higher selectivity (around 40 %),
that is probably due to the more favourable
entropy to close a five-atoms ring

Quote
In the di-(poly-)carboxylic acids
anodic oxidation which has been performed
with a partial (10-20 %) neutralization, a high
loco-selectivity has been noticed; only the
most acidic carboxyl group reacts. From citric
acid acetone is obtained (by double
decarboxylation of the b-ketonic acid formed);
from malic acid succindialdehyde principally
results by an interesting succession of non-
Kolbe and Kolbe reactions of the two carboxyl
groups.

The complete article is here, but I can only locate it through google cache. It doesn't appear to be available on their site anymore:
http://docs.google.com/viewer?a=v&q=cache:CECdvHBd6XcJ:www.cael.pub.ro/SiteulCAEL/cicic/chorg/ACIDMA~2.pdf+ANODIC+OXIDATION+OF+MALIC+ACID+G.+Stanciu+,+E.M.+Ungureanu&hl=nl&gl=be&pid=bl&srcid=ADGEESjeCb5wnQbob5dmym3jnaM2XQihyGSFhv2WhOu-Jc_XQvxasEKEyBCbSCCrixee_QyrY4Au_l7admykipcJbY0497Fs9LJC3bi-egpgM7Fx9Hm6jrACAEtLycHYY5ObHTqFuTaJ&sig=AHIEtbTuNArJjSHPqFkF8nyowUZkKsUf7g
It is perhaps the narcotic. Hyoscine affects certain people very oddly. One cannot be sure. Sometimes, these cases take strange forms. The victim becomes in a sense, 'mediumistic', a vehicle for all the intangible forces in operation around her.

java

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #14 on: November 05, 2011, 04:26:05 PM »
Reference Information

....here is the article in a pdf format.



ANODIC OXIDATION OF MALIC ACID
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

fresh1

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #15 on: November 05, 2011, 09:09:37 PM »
                              using yeast to selectively reduce ketones?

                        Jayasinghe. L.Y,,Smallridge.A.J,,& Trewhella.M.A 1993
   
           "The yeast mediated reduction of ethyl acetoacetate in petroleum ether"
« Last Edit: November 06, 2011, 10:40:02 PM by fresh1 »
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beanhead

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Re: Bet you can't post awesome OTC reagents/synthesis I've never seen before
« Reply #16 on: November 06, 2011, 08:47:56 PM »
Quote from: Sydenhams chorea on October 19, 2011, 09:11:57 PM
Also from memory:

sugar + acid + heat --> levulinic acid, ester when done in alcoholic environment

reduction gives  gamma-valerolactone (weaker version of GHB) but perhaps more interestingly: Fisher indole synthesis with phenylhydrazine gives 2-methylindoleacetic acid.

no way! a toned down version of GHB?

Yay something new and easy to pursue, thanks :)
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