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Topic: Experimental Considerations  (Read 1464 times)

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Offline Guitarmaniac86

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Experimental Considerations
« on: May 04, 2015, 11:42:05 AM »
I require some advice on how to do the following reaction.

I cannot go into structural detail due to confidentiality reasons. I reacted an α,β unsaturated methyl ester with benzylmercaptan to form the 1,4-addition product. Now I want to remove the benzyl group to leave a tertiary SH and I am planning on doing this with sodium in liquid ammonia (lit prep) however, a lecture bottle of ammonia gas is £900+ from Sigma and I dont want to spend that kind of money.

I need the gas to be anhydrous so I was wondering if I could just take ammonium carbonate/sulphate/hydroxide heat it to decompose it, pass that gas into an empty conical which is connected to my reaction vessel at -78°C to condense the gas. 

The set up I envisage is as follows:

http://i.imgur.com/o3J1dC6.jpg

If anyone has done this please could I get some pointers, thanks!
« Last Edit: May 04, 2015, 12:40:05 PM by Arkcon »
Don't believe atoms, they make up everything!

Offline Dan

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Re: Experimental Considerations
« Reply #1 on: May 04, 2015, 12:58:32 PM »
My research: Google Scholar and Researchgate

Offline Guitarmaniac86

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Re: Experimental Considerations
« Reply #2 on: May 04, 2015, 01:10:43 PM »
Awesome thanks!
Don't believe atoms, they make up everything!

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