3-Chloropropionyl chloride → HCID 18522615, compound

Participants

Reaction Conditions

Reaction Steps

Into a glass-made, 500-mL reaction vessel equipped with a stirrer, the 2-(2′-mercaptoethyl)-1,3-dithiolane produced in Synthesis Example 2 (100 g, 0.60 mole) was weighed, to which 3-chloropropionic acid chloride (80 g, 0.63 mole) was added dropwise at 40° C. over 15 minutes. After the contents were reacted further under stirring at 40° C. for 8 hours, toluene (200 g) was added to the reaction mixture to dissolve the same. The resulting solution was transferred into a separating funnel, in which the solution was washed three times with a 3 wt. % aqueous solution of sodium hydrogen carbonate (300 g). After the organic layer (toluene solution) was washed with purified water (300 g) until the water layer became neutral, the organic layer was taken out, and toluene was then distilled off under reduced pressure to afford 2-[2-(3-chloropropionylthio)ethyl]-1,3-dithiolane (127 g).

Provenance & Evidence