反应详情

To a 3-liter flask were added 1170 ml. of 1,2-dichloroethane, 308 g. of dimethylaminothioacetamide, hydrochloride, 279 g. of 1,3-dichloropropanone and 370 g. of sodium bicarbonate. The mixture was stirred for 8 hours, and 500 ml. of additional 1,2-dichloroethane was added and the mixture stirred for a short time more. It was then filtered, the filter cake was washed with 670 ml. of 1,2-dichloroethane, and the filtrates were combined and chilled in an ice bath. To the filtrate was added 157 ml. of thionyl chloride, dropwise, with good stirring. It was then warmed and stirred overnight at ambient temperature, and then for 30 minutes at 65°-70°. It was then cooled and filtered, and the solids were washed with 500 ml. of additional 1,2-dichloroethane and dried to obtain 427 g. of the desired product. The product was confirmed to be substantially identical to the product of Example 5 by nuclear magnetic resonance analysis.

1. additionTo a 3-liter flask were added 1170 ml
2. stirringthe mixture stirred for a short time more
3. filtrationIt was then filtered
4. washthe filter cake was washed with 670 ml
5. temperaturechilled in an ice bath
6. additionTo the filtrate was added 157 ml
7. temperatureIt was then warmed
8. stirringstirred overnight at ambient temperature
9. waitfor 30 minutes at 65°-70°
10. temperatureIt was then cooled
11. filtrationfiltered
12. washthe solids were washed with 500 ml
13. dry with materialof additional 1,2-dichloroethane and dried
14. customto obtain 427 g