反应详情

23.2 g (58.8 mmol) of 5-(o-fluorophenyl)-1,3-dihydro-7-iodo-3-methyl-2H-1,4-benzodiazepin-2-one and 10 g (0.11 mol) of copper (I) cyanide in 250 ml of dimethylformamide are heated at 150° for 2 hours under argon. After cooling, 700 ml of water are added to the mixture and the resulting precipitate is filtered off. This is dissolved in 1 l of water/ethylenediamine (1:1) and extracted with 1 l of methylene chloride; the separated aqueous phase is extracted a further twice with methylene chloride. The combined organic extracts are washed with water, dried and evaporated. The residue gives, from cyclohexane, 5-(o-fluorophenyl)-2,3-dihydro-3-methyl-2-oxo-1H-1,4-benzodiazepine-7-carbonitrile of melting point 216°.

1. temperatureAfter cooling
2. filtrationthe resulting precipitate is filtered off
3. dissolutionThis is dissolved in 1 l of water/ethylenediamine (1:1)
4. extractionextracted with 1 l of methylene chloride
5. extractionthe separated aqueous phase is extracted a further twice with methylene chloride
6. washThe combined organic extracts are washed with water
7. customdried
8. customevaporated