反应详情

温度

20 °C

A two-phase mixture containing 6.0 g (0.0495 mol) dl-α-methylbenzylamine and 8.0 g (0.05 mol) 25% NaOH in 50 ml water was stirred rapidly at 0°-10° C. while 4.0 g (0.05 mol) carbon disulfide was added dropwise over 2-3 minutes. The mixture was stirred and allowed to warm to 20° C. over a one hour period. To this stirred slurry was added 9.0 g (0.05 mol) 1,1,2,3-tetrachloropropene in one portion. A yellow two phase mixture resulted and the temperature slowly rose to a maximum of 28° C. The mixture was heated gently to 45°-50° C. for three hours, then let cool and extracted with 300 ml ethyl ether. The ether solution was washed with two, 50 ml portions of water, treated with activated charcoal and MgSO4, filtered through Hy-flo and evaporated in vacuo below 40°/<1 torr to give 14.9 g (88%) of a light orange oil.

1. additionwas added dropwise over 2-3 minutes
2. customA yellow two phase mixture resulted
3. customslowly rose to a maximum of 28° C
4. temperatureThe mixture was heated gently to 45°-50° C. for three hours
5. temperaturelet cool
6. extractionextracted with 300 ml ethyl ether
7. washThe ether solution was washed with two, 50 ml portions of water
8. additiontreated with activated charcoal and MgSO4
9. filtrationfiltered through Hy-flo
10. customevaporated in vacuo below 40°/<1 torr