反应详情

温度

0 °C

27 g of chlorosulfuric acid were slowly added at 0° C to a mixture of 12 g of ethylene sulfide and 200 ml of methylene chloride and the mixture was stirred at 0° C for 10 minutes and was then cooled to -20° C. A mixture of 32.6 g of N-methyl-N'-(3,4-dichlorophenyl)-urea in 210 ml of pyridine was added to the reaction mixture after which the temperature returned to 0° C. The mixture was stirred at 0° C for 10 minutes and was then poured into a mixture of ice, water, hydrochloric acid and methylene chloride. The mixture was stirred for 30 minutes and the decanted organic phase was washed, dried, filtered and concentrated to dryness under reduced pressure. The residue was chromatographed over silica gel and the product was eluted witn 9-1 benzene-ethyl acetate mixture and was crystallized from isopropyl ether to obtain 10 g of N-(2-chloroethylthio)-N-methyl-N'-(3,4-dichlorophenyl)-urea melting at 62° C.

1. temperaturewas then cooled to -20° C
2. additionwas added to the reaction mixture after which the temperature
3. customreturned to 0° C
4. stirringThe mixture was stirred at 0° C for 10 minutes
5. stirringThe mixture was stirred for 30 minutes
6. washthe decanted organic phase was washed
7. customdried
8. filtrationfiltered
9. concentrationconcentrated to dryness under reduced pressure
10. customThe residue was chromatographed over silica gel
11. washthe product was eluted witn 9-1 benzene-ethyl acetate mixture
12. customwas crystallized from isopropyl ether