反应详情

温度

150 °C

A mixture of 6-bromo-3,4-difluoro-2-methylthiomethylaniline (99 g), HMPA (130 g) and copper cyanide (48 g) is heated at 150° C. for 4 hours. After cooling, the reaction mixture is poured into a solution of ethylenediamine (50 ml) in water (500 ml), and the mixture is heated at 60° C. for one hour. After cooling, the mixture is extracted with ethyl acetate, and the extract is dried over magnesium sulfate and concentrated. The resulting residue is purified by silica gel column chromatography (solvent, dichloromethane:n-hexane=1:1), and the product is recrystallized from ethanol to give 2-amino-4,5-difluoro-3-methylthiomethylbenzonitrile (28 g), as a white crystal, m.p. 109°-110° C.

1. temperatureAfter cooling
2. temperaturethe mixture is heated at 60° C. for one hour
3. temperatureAfter cooling
4. extractionthe mixture is extracted with ethyl acetate
5. dry with materialthe extract is dried over magnesium sulfate
6. concentrationconcentrated
7. customThe resulting residue is purified by silica gel column chromatography (solvent, dichloromethane:n-hexane=1:1)
8. customthe product is recrystallized from ethanol