HRID2267095

反应详情

EQUATION

反应方程式

HRID 2267095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

The compound 21 (75.2 g, 222 mmol) and copper (I) iodide (21.1 g, 111 mmol) were dissolved in dimethylformamide (750 ml), a 28% sodium methoxide-methanol solution (216 ml, 888 mmol) was added, and the mixture was stirred at 105° C. for 100 minutes. After cooling, ice-water (800 ml) was added, and unnecessary matter were filtered. To the solution was added 2M hydrochloric acid (443 ml), and crystals were collected by filtration. N-(4-fluorobenzyl)-4-hydroxy-5-methoxy-6-methylnicotinamide 22 (56.0 g, 870%) was obtained as a colorless crystal.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationunnecessary matter were filtered
  3. additionTo the solution was added 2M hydrochloric acid (443 ml), and crystals
  4. filtrationwere collected by filtration