反应详情

A solution of 12.1 g of propyl N-chlorosulphenyl-N-methylcarbamate in 20 ml of diethyl ether was added over 20 minutes to a stirred solution of 18.3 g of 31, and 7 g of triethylamine in 70 ml of the same solvent, the temperature of the mixture being maintained at 15°-20° C. with cooling. Stirring was continued at room temperature for a further 11/2 hours. The reaction mixture was then diluted with 200 ml of diethyl ether, washed with water, dried and stripped of solvent. The residue was added to 100 ml of toluene, then the toluene was evaporated under reduced pressure to leave 32, in crude form as a pale brown oil.

1. temperaturethe temperature of the mixture being maintained at 15°-20° C.
2. temperaturewith cooling
3. customwas continued at room temperature for a further 11
4. custom2 hours
5. washwashed with water
6. customdried
7. additionThe residue was added to 100 ml of toluene
8. customthe toluene was evaporated under reduced pressure