HRID68943

反应详情

EQUATION

反应方程式

HRID 68943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carbonitrile (1.0 g) and Raney nickel (3.0 g) were suspended in formic acid (10 ml), and the mixture was stirred at 100° C. for 2 hours. The reaction mixture was filtered to remove insoluble matter, and the filtrate was condensed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:50→20:80). The purified product was condensed under reduced pressure to give the title compound (0.92 g) as a yellowish-white solid (yield=92%).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customto remove insoluble matter
  3. customcondensed under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:50→20:80)
  5. customcondensed under reduced pressure