Another similar synthesis, generating sulfur chloride in situ:
Mix quickly and thoroughly 205-215 g of pulverized fine NaOAc and 10g dry sulfur powder, the mixture is quickly transferred to a wide-mouth 1 liter RBF and wetted w/25 ml acetic anhydride. Into the flask through the rubber cork extend 1) a wide tube for chlorine in-flow 2) an overhead stirrer, which is sealed with the aid of a piece of rubber tubing greased with vaseline and 3) an out-leading tube for excess Cl2 release. The flask is immersed in an ice-bath. Chlorine is initially passed in very carefully, with frequent stirring or shaking, over the passage of time the rxn gets hotter and more and more liquid, so the stirrer may bee after some time rotated with a motor. Chlorine stream should bee regulated so that almost all of it is absorbed. When the reaction mixture stops heating and Cl2 is no longer taken up, the rxn contents are distilled in vacuo at oil bath temp ~150-180°C, then redistilled at ordinary pressure, collecting the fraction boiling between 132 and 142°C. Yield ~90%.
Has anyone tried this without using the AA as a pre-wetting agent, Would it work ok, the first time around, but with a lower yield?, say if you substituted GAA instead,.
Sure would be nice.!
hm