反应详情

温度

70 °C

882 g (4.14 mols) of 4-(cyclopropyl-methyl-methylene)-N-methylrhodanine (as an E/Z mixture) are introduced into a solution of 712 g (17.8 mols) of sodium hydroxide in 4.4 l of water. After the addition of 7 ml of alkylaryl polyglycol ether, the mixture is stirred at 70° C. until complete dissolution occurs (about 16 hours). 438 g (4.14 mols) of thiocarbohydrazide and 115 ml of 1-decanol are then added, the mixture is stirred for one hour at 70° C., and 1525 ml of acetic acid are rapidly added dropwise, causing the reaction product to precipitate. The mixture is stirred at 80° C. for a further 2 hours, allowed to cool to room temperature and the precipitate is filtered off with suction, washed several times with water and also with petroleum ether and dried at 70° C. 725 g (82.6% of theory) of the above compound of melting point 142°-143° C. are obtained.

1. custom(about 16 hours)
2. stirringthe mixture is stirred for one hour at 70° C.
3. customto precipitate
4. stirringThe mixture is stirred at 80° C. for a further 2 hours
5. temperatureto cool to room temperature
6. filtrationthe precipitate is filtered off with suction
7. washwashed several times with water
8. dry with materialalso with petroleum ether and dried at 70° C
9. custom725 g (82.6% of theory) of the above compound of melting point 142°-143° C. are obtained