HRID490262

反应详情

EQUATION

反应方程式

HRID 490262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

A solution of 2-(2-{1-[1-(3-benzyl-7-chloro-4-oxo-3,4-dihydro-quinazolin-2-yl)-2-methyl-propyl]-2-p-tolyl-1H-imidazol-4-yl}-ethyl)-isoindole-1,3-dione (278 mg, 0.423 mmol) and anhydrous hydrazine (98 mg, 3.06 mmol) in EtOH (12 mL) was refluxed for 3.0 h. The reaction was cooled to 5° C. and a white precipitate was filtered off. The filtrate was concentrated in vacuo and purified by flash chromatography (silica gel, 90:9:1 methylene chloride:methanol:ammonium hydroxide as eluent) to provide the title compound as a white solid (98.2 mg, 45%). MS(ES+) m/e 526 [M+H]+.

WORKUP

后处理

  1. filtrationa white precipitate was filtered off
  2. concentrationThe filtrate was concentrated in vacuo
  3. custompurified by flash chromatography (silica gel, 90:9:1 methylene chloride:methanol:ammonium hydroxide as eluent)