反应详情

Beneath a solution of 20 g of trans-decahydroquinoline in 100 ml of benzene is introduced a layer consisting of a solution of 5.8 g of sodium hydroxide in 100 ml of water. While stiring vigorously and cooling to 5°-10°C, 20 g of chlorothioformic acid allyl ester are then added dropwise to the mixture. Upon completion of the reaction, stirring is continued for 3 hours, the phases are separated, the benzene phase is washed until neutral, dried, and the benzene evaporated in vacuo. The residual oil is distilled in vacuo to yield 24 g (70% of theory) of 1-(allylthiocarbonyl)-trans-decahydroquinoline (b.p. 110°-116°C/0.2 Torr).

1. temperaturecooling to 5°-10°C
2. customUpon completion of the reaction
3. customthe phases are separated
4. washthe benzene phase is washed until neutral,
5. customdried
6. customthe benzene evaporated in vacuo
7. distillationThe residual oil is distilled in vacuo