HRID892154

反应详情

EQUATION

反应方程式

HRID 892154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Heated (60° C.) a mixture of 2-cyanomethoxy-3-methylbenzyl bromide (10.2 g, 42.7 mmoles, example 24), resorcinol (18.8 g, 171 mmoles), and potassium carbonate (47.2 g, 342 mmoles) in acetonitrile (140 mL) for two hours. The reaction is diluted with ether and washed three times with distilled water, once with brine, and dried over MgSO4. The organic layer is isolated and concentrated, and the resulting residue is purified by column chromatography (silica, 5% EtOAc/CH2Cl2) to yield the title compound as a white crystalline solid. MS(EI) 269 (M)+.

WORKUP

后处理

  1. washwashed three times with distilled water
  2. dry with materialonce with brine, and dried over MgSO4
  3. customThe organic layer is isolated
  4. concentrationconcentrated
  5. customthe resulting residue is purified by column chromatography (silica, 5% EtOAc/CH2Cl2)