2-methanesulfonylethane-1-thiol synthesis

Yield:24517-45-1 80%

Reaction Conditions:

with hydrogen sulfide in toluene at 60; for 1 h;Inert atmosphere;

Steps:

5

A 100 mL four-necked flask was charged with 1.5 g of trimethylamine-based quaternary ammonium base catalyst (DS = 0.44) Toluene (30 mL), stirred for 30 min, and then heated to 60 ° C. Then, hydrogen sulfide gas (0.6 L / h) was introduced into the reaction solution, And dropping methyl vinyl sulfone solution (5g diluted to 20mL); reaction for some time, The liquid phase, liquid quality and temperament analysis were carried out until the liquid phase test showed that the product content was not changed after lh, the hydrogen sulfide gas was stopped, nitrogen was cooled to room temperature, and the reaction solution was filtered and the filtrate was decompressed Distillation, collecting products with a boiling point of 105-107 ° C. The results of liquid and liquid analysis show that the conversion of methyl vinyl sulfone can reach 90%, the selectivity of methyl mercaptoethyl sulfone Was 92% and the yield was 80%.

References:

CN104276987,2016,B Location in patent:Paragraph 0048-0049