HRID1976272

反应详情

EQUATION

反应方程式

HRID 1976272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

50 g (0.118 mol of 3(R,S)-bromo-1-methyl4-(2,4,6-trimethoxyphenyl)-1,2,3,6-tetrahydropyridine hydrobromide (VI) were heated under reflux for 2 h in 100 ml of water. The reaction mixture was then cooled to 20° C. and adjusted to pH 12.5 by dropwise addition of 30 ml of 30% strength sodium hydroxide solution. After a short time, a pale brown precipitate crystallized out. The mixture was stirred at 5-10° C. for a further 1 h, and the precipitated product was filtered off with suction and washed with 30 ml of water. The crude product was then stirred with 20 ml of acetone, filtered off with suction and dried in vacuo.

WORKUP

后处理

  1. customAfter a short time, a pale brown precipitate crystallized out
  2. filtrationthe precipitated product was filtered off with suction
  3. washwashed with 30 ml of water
  4. stirringThe crude product was then stirred with 20 ml of acetone
  5. filtrationfiltered off with suction
  6. customdried in vacuo