反应详情

350 parts of triethylamine are added dropwise to a mixture of 178 parts of chloroacetyl chloride, 104 parts of malonodinitrile and 900 parts of dimethylformamide, while cooling with ice. The solution is stirred for a further hour at room temperature, after which it is introduced into a mixture of 294.5 parts of a 40% strength aqueous ammonium sulfide solution, 1000 parts of ice and 1000 parts of water, and the reaction mixture is stirred for a further 3 hours at room temperature. The precipitate formed is filtered off under suction, washed with water and dried. 137 parts (62% of theory) of 2-amino-3-cyano-4-hydroxythiophene are obtained.

1. temperaturewhile cooling with ice
2. stirringthe reaction mixture is stirred for a further 3 hours at room temperature
3. customThe precipitate formed
4. filtrationis filtered off under suction
5. washwashed with water
6. customdried