反应详情

A mixture of 118 g. of dimethylaminothioacetamide, 92.4 g. of sodium bicarbonate, 140 g. of 1,3-dichloropropanone and 600 ml. of 1,2-dichloroethane was stirred at ambient temperature for 24 hours, and was then filtered. To the filtrate, at ice-bath temperature, was added 131 g. of thionyl chloride, dropwise. One hundred ml. of additional 1,2-dichloroethane was added, and the mixture was stirred for 2 hours at ambient temperature and then for 1 hour under reflux. The mixture was then chilled overnight, warmed to ambient temperature and filtered. The filter cake was washed with 200 ml. of 1,2-dichloroethane and blown dry, and the solids were dried overnight under vacuum to obtain 202.5 g. of the desired product, substantially identical to the product of Example 5.

1. additionA mixture of 118 g
2. filtrationwas then filtered
3. additionTo the filtrate, at ice-bath temperature, was added 131 g
4. additionof additional 1,2-dichloroethane was added
5. temperaturefor 1 hour under reflux
6. temperatureThe mixture was then chilled overnight
7. temperaturewarmed to ambient temperature
8. filtrationfiltered
9. washThe filter cake was washed with 200 ml
10. dry with materialof 1,2-dichloroethane and blown dry, and the solids were dried overnight under vacuum
11. customto obtain 202.5 g