HRID1179669

反应详情

EQUATION

反应方程式

HRID 1179669 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

N-(6-Methoxy-pyridin-3-yl)-benzamide (2.38 g, 10.4 mmol) was dissolved in a mixture of tetrahydrofuran and diethyl ether. HCl-gas was bubbled into the solution for 5 minutes. More diethyl ether was added and the white precipitate was collected by suction, washed twice with diethyl ether and heated in a kugelrohr apparatus at 180° C. for 0.5 hours. The solid material was crystallised from methanol:water, washed twice with water and dried overnight in a vacuum oven, yielding the title compound (1.19 g, 53% yield) as a grey solid.

WORKUP

后处理

  1. customwas bubbled into the solution for 5 minutes
  2. additionMore diethyl ether was added
  3. customthe white precipitate was collected by suction
  4. washwashed twice with diethyl ether
  5. customThe solid material was crystallised from methanol
  6. washwater, washed twice with water
  7. customdried overnight in a vacuum oven