Reacción #311981

Ecuación de reacción

sodium hydroxide

thiophosgene

chloroform

cyclohexyl mercaptan

→

cyclohexyl dichloromethyl disulfide

Rendimiento 67.2%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   Otrothe temperature less than 8° C
3. 3
   workup.ADDITIONWhen the addition
4. 4
   Otrothe chloroform layer was separated
5. 5
   Secadodried over calcium chloride
6. 6
   OtroThe solvent was evaporated
7. 7
   workup.DISTILLATIONthe residue was distilled under reduced pressure

Procedimiento

To a solution of 20.0 g (0.17 mole) of thiophosgene in 100 ml. of chloroform cooled to 0° C. was added dropwise with stirring 20.2 g (0.17 mole) of cyclohexyl mercaptan. To this mixture was added dropwise a solution of 2.5 g of sodium hydroxide in 25 ml. of water at such a rate as to keep the temperature less than 8° C. When the addition was complete, the chloroform layer was separated and dried over calcium chloride. The solvent was evaporated, and the residue was distilled under reduced pressure to give 26.4 g of yellow cyclohexyl dichloromethyl disulfide, b.p. 118°-125° C. (5 Torr.)

Fuente