反应 #53361

反应方程式

starting material XXIV

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

triethyl orthoformate

hydrochloric acid

→

title compound

收率 75.0%

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

收率 75.0%

反应条件

后处理

1. 1
   浓缩concentrated in vacuum
2. 2
   workup.STIRRINGThe residue was stirred with water
3. 3
   过滤the precipitated crystals were filtered off
4. 4
   洗涤washed with water
5. 5
   其他recrystallized from 2-methoxyethanol

实验过程

A mixture of 1.50 g (3.91 mmol) of the starting material XXIV and 15 ml of triethyl orthoformate in the presence of 0.05 ml of 36% hydrochloric acid was stirred at 110° C. for 30 min, then concentrated in vacuum. The residue was stirred with water, the precipitated crystals were filtered off, washed with water and recrystallized from 2-methoxyethanol to yield 1.15 g (75%) of the title compound; Mp.: 190-196° C.

来源