HRID577463

反应详情

EQUATION

反应方程式

HRID 577463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 2-hydroxy-4,6-dimethylnicotinonitrile (5.3 g, 36 mmol), benzyl chloride (5.7 mL, 45 mmol), silver(I)oxide (9.2 g, 40 mmol) and toluene (50 mL) were heated at 110° C. in a sealed tube for 20 hours. The mixture was cooled to room temperature and the solids were filtered and rinsed with dichloromethane. The filtrate was concentrated under vacuum and purified by column chromatography (40% EtOAc/Heptane) to give 2-(benzyloxy)-4,6-dimethylnicotinonitrile (Cpd II, 8.1 g, 94% yield) as a white solid.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationthe solids were filtered
  3. washrinsed with dichloromethane
  4. concentrationThe filtrate was concentrated under vacuum
  5. custompurified by column chromatography (40% EtOAc/Heptane)