HRID1504135

反应详情

EQUATION

反应方程式

HRID 1504135 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(2,2-Dihydroxyethyl)-2-methyl-5H-furo[3,2-c]pyridine-4-one(0.21 g) and acetic acid(0.1 ml) were added to a 1,2-dichloroethane solution(15 ml) of 1-ethyl-3,3,5-trimethyl-7-{[(pyridin-4-ylmethyl)amino]methyl}-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione(0.38 g), and the mixture was stirred for 30 minutes at room temperature. Sodium triacetoxy borohydride(0.42 g) was added, and the mixture was stirred at room temperature overnight. The reaction mixture was condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate: methanol=1:0→4:1). The purified product was condensed under reduced pressure, and the residue was recrystallized from ether to give the title compound(0.47 g) as a white powder.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature overnight
  2. customcondensed under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (ethyl acetate: methanol=1:0→4:1)
  4. customcondensed under reduced pressure
  5. customthe residue was recrystallized from ether