HRID1485381

反应详情

EQUATION

反应方程式

HRID 1485381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a THF (5 ml) solution of 6-(4-chlorophenyl)-1,4,4-trimethyl-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-5(6H)-one of (51 mg, 0.14 mmol) was added BH3-THF complex (1 mL, 1M in THF) drop-wise at 0° C. The resulting mixture was heated at reflux overnight, then the mixture was concentrated in vacuo and the residue was purified by Prep-TLC (silica-gel, DCM:methanol=10:1) to give 6-(4-chlorophenyl)-1,4,4-trimethyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepine as a white solid (5.0 mg, yield 10.4%).

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. concentrationthe mixture was concentrated in vacuo
  4. customthe residue was purified by Prep-TLC (silica-gel, DCM:methanol=10:1)