Sodium Hydroxide → HCID 20542102, compound

Participants

Reaction Steps

62.7 g (0.2 mol) of crude rac-5-(o-fluorophenyl)-1,3-dihydro-3-methyl-7-nitro-2H-1,4-benzodiazepin-2-one in 1 l of concentrated hydrochloric acid is treated portionwise while stirring with a total of 135.5 g (0.6 mol) of tin chloride, stirred at room temperature for 2 hours and the mixture is neutralised in the cold with 10 N sodium hydroxide. The aqueous phase is extracted with a total of 8 l of methylene chloride/ethanol (4:1), the combined organic extracts are washed with saturated sodium chloride solution, dried and evaporated. From ether there is obtained 7-amino-5-(o-fluorophenyl)-1,3-dihydro-3-methyl-2H-1,4-benzodiazepin-2-one of melting point 270°.

Provenance & Evidence