反应详情

A solution of 5.0 g (16.68 mmol) of 7-amino-5-(o-chlorophenyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one and 1.74 g (22.02 mmol) of hydroxylamine hydrochloride in 50 ml of pyridine is heated to reflux for 2 hours under argon. After cooling, the mixture is taken up in 600 ml chloroform/ethanol (4:1) and washed with 250 ml of water. The aqueous phase is adjusted to pH 8, saturated with sodium chloride and extracted with chloroform overnight in a perforator. After drying and evaporating the solvent, the residue is suspended in hot tert.-butyl methyl ether and filtered off. There is obtained 2,4'-diamino-2'-[o-chloro-α-(hydroxyimino)benzyl]-N-methylacetanilide of melting point 150° (decomposition).

1. temperatureto reflux for 2 hours under argon
2. temperatureAfter cooling
3. washwashed with 250 ml of water
4. extractionextracted with chloroform overnight in a perforator
5. customAfter drying
6. customevaporating the solvent
7. filtrationfiltered off