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To a 1000 ml. flask were added 77 g. of dimethylaminothioacetamide, hydrochloride, 70 g. of 1,3-dichloropropanone, 92.4 g. of sodium bicarbonate and 350 ml. of 1,2-dichloroethane. The mixture was stirred at ambient temperature for 26 hours and filtered, and the filter cake was washed with 118 ml. of 1,2-dichloroethane. The filtrates were combined and cooled in an acetone-ice bath. To the filtrate was added, dropwise, 39.5 ml. of thionyl chloride at a temperature between 13° and 18°. The mixture was stirred at 20° for 30 minutes, then heated to 50°. An additional 100 ml. of 1,2-dichloroethane was added, and the mixture was stirred for 30 minutes at 60°. It was then cooled to ambient temperature, and 82 ml. of deionized water was added. The layers were separated, and the organic layer was extracted with 28 ml. and 14 ml. portions of deionized water. The aqueous layers were combined, and it was confirmed by tlc that the desired product had been collected in the aqueous layers.

1. additionflask were added 77 g
2. filtrationfiltered
3. washthe filter cake was washed with 118 ml
4. temperaturecooled in an acetone-ice bath
5. additionTo the filtrate was added
6. customat a temperature between 13° and 18°
7. stirringThe mixture was stirred at 20° for 30 minutes
8. temperatureheated to 50°
9. additionof 1,2-dichloroethane was added
10. stirringthe mixture was stirred for 30 minutes at 60°
11. temperatureIt was then cooled to ambient temperature
12. additionof deionized water was added
13. customThe layers were separated
14. extractionthe organic layer was extracted with 28 ml
15. customhad been collected in the aqueous layers