反应详情

A mixture of 5.33 g of 2-acetoxythioacetamide prepared according to Example 2, 5.21 g of 1,3-dichloroacetone, 6.88 g of sodium bicarbonate and 20 ml of 1,2-dichloroethane was stirred at room temperature for 87 hours. The mixture was filtered to remove insoluble inorganics and concentrated under reduced pressure to an oil. The oil was taken up in 4 mls of 1,2-dichloroethane and 25 mils of cyclohexane added dropwise. The slurry was stirred for 1 hour at 0° C. and then filtered. The precipitate was washed with cyclohexane and dried at room temperature under reduced pressure. The product 2-acetoxymethyl-4-chloromethyl-4-hydroxy-thiazoline was obtained in 92% yield (8.25 g).

1. customprepared
2. filtrationThe mixture was filtered
3. customto remove insoluble inorganics
4. concentrationconcentrated under reduced pressure to an oil
5. addition25 mils of cyclohexane added dropwise
6. stirringThe slurry was stirred for 1 hour at 0° C.
7. filtrationfiltered
8. washThe precipitate was washed with cyclohexane
9. customdried at room temperature under reduced pressure