HRID433212

反应详情

EQUATION

反应方程式

HRID 433212 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 6-hydroxymethyl-pyridin-3-ol hydrochloride (1:1) (6.29 g, 38.9 mmol), 3-fluorobenzyl bromide (8.1 g, 42.8 mmol), potassium carbonate (10.76 g, 77.9 mmol) and 2-butanone (200 ml) was heated to 80° C. for 5 h. After cooling, water was added, and the mixture extracted with ethyl acetate. After drying of the organic layer with MgSO4, filtration and evaporation, the residue was purified by chromatography (SiO2, CH2Cl2—MeOH 95:5) to give the title compound as a brown solid (6.12 g, 67%). MS: m/e=234.3 (M+H+).

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe mixture extracted with ethyl acetate
  3. dry with materialAfter drying of the organic layer with MgSO4, filtration and evaporation
  4. customthe residue was purified by chromatography (SiO2, CH2Cl2—MeOH 95:5)