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Chemistry Forums for Students => Organic Chemistry Forum => Organic Chemistry Forum for Graduate Students and Professionals => Topic started by: muse on October 25, 2017, 03:38:47 PM

Title: Reaction in autoclave tube
Post by: muse on October 25, 2017, 03:38:47 PM

Hi

I'm planning to synthesis a vinylsulfide from vinyl bromide and a thiol. I found a reference http://pubs.acs.org/doi/abs/10.1021/jo0619736 (http://pubs.acs.org/doi/abs/10.1021/jo0619736) where this is done in an autoclave tube at 105°C in THF and EtONa.
I'm have never done reactions in an autoclave tube. Could anyone guide me on what sort of equipment is needed and important safety aspects to be aware of?
Could a microwave be used instead or is it possible to perform it in a RBF under reflux with extremely good cooling (vinyl bromide Bp=15.8C)?

-M

Title: Re: Reaction in autoclave tube
Post by: phth on October 25, 2017, 10:25:44 PM

Autoclave is just a high pressure Rxn.  You could use a hydrogenation bottle in an oil bath also: https://us.vwr.com/store/product/4831644/pressure-tubes-with-ace-thred-ace-glass

I think a microwave tube could work if it can sustain high pressure (test this with argon/N20)..