反应详情

温度

0 °C

3.1 g (0.07 mol) of lithium hydroxide hydrate are added in portions, at 0° C., to 16.7 g (0.07 mol) of 3-trichloromethyl-5-chloro-1,2,4-thiadiazole and 11.8 g (0.07 mol) of hydroxyacetic acid N-methyl-N-cyclohex-1-enylamide in 100 ml of methyl isobutyl ketone, and the mixture is stirred for 30 minutes at 0° C. and then overnight at 25° C. After water has been added, the reaction product which separates out as a solid is filtered off under suction, washed and dried. 22.0 g (84.8% of theory) of 3-trichloromethyl-1,2,4-thiadiazol-5-yl-oxyacetic acid N-methyl-N-cyclohexen-1-yl-amide are obtained in the form of beige-colored crystals of melting point 78° C.

1. customovernight
2. customat 25° C
3. filtrationis filtered off under suction
4. washwashed
5. customdried