반응 #53338

반응 방정식

compound XXIII

(±)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbonitrile

sodium acetate

hydroxylamine hydrochloride

→

title compound

수율 100.0%

(±)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbamidoxime

수율 100.0%

용매

2-methoxyethanol

반응 조건

후처리

1. 1
   농축concentrated in vacuum
2. 2
   workup.ADDITIONThe residue was treated with water
3. 3
   여과the precipitated crystals were filtered off
4. 4
   세척washed with water

실험 절차

A mixture of 2.80 g (8.0 mmol) of compound XXIII, 30 ml of 2-methoxyethanol, 0.84 g (10 mmol) of sodium acetate and 0.60 g (8.8 mmol) of hydroxylamine hydrochloride was stirred for 0.5 h, then concentrated in vacuum. The residue was treated with water, the precipitated crystals were filtered off and washed with water to yield 3.05 g (100%) of the title compound, Mp.: 138-145° C.

출처