反应详情

10 g of 2-chloro-4-fluorobenzyl cyanide are dissolved at a temperature of -10° C., with stirring, in 85 ml of concentrated sulfuric acid, in the process of which a fine light-brown suspension is formed. There are then slowly added dropwise at -20° C., with stirring, 5 ml of fuming nitric acid. After completion of the addition, stirring is continued for a further half hour, the temperature rising to 0° C. The reaction mixture is poured onto 500 g of ice, and the substance which precipitates is extracted with methylene chloride. The methylene chloride phase is dried over sodium sulfate, and concentrated by evaporation to leave 10.5 g of 2-chloro-4-fluoro-5nitrobenzyl cyanide in the form of white crystals having a melting point of 67°-68° C.

1. customis formed
2. additionThere are then slowly added dropwise at -20° C.
3. additionAfter completion of the addition
4. stirringstirring
5. customrising to 0° C
6. customthe substance which precipitates
7. extractionis extracted with methylene chloride
8. dry with materialThe methylene chloride phase is dried over sodium sulfate
9. concentrationconcentrated by evaporation