HRID860913

反应详情

EQUATION

反应方程式

HRID 860913 的结构方程式

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

Dodecanethiol (122 g), venlafaxine (111 g), and a methanolic solution of sodium methanolate (30%, 90 g) and PEG 400 are heated to 190° C. The methanol is distilled off and the solution is stirred for 2 hours at 190° C. Then the temperature is lowered, 2-propanol (450 g) is added and the pH is adjusted to 9.5 with aqueous HCl. The precipitate is collected by suction filtration, and the cake is washed with 2-propanol, toluene, 2-propanol and water. The wet O-desmethylvenlafaxine is dried in vacuo.

WORKUP

后处理

  1. distillationThe methanol is distilled off
  2. addition2-propanol (450 g) is added
  3. filtrationThe precipitate is collected by suction filtration
  4. washthe cake is washed with 2-propanol, toluene, 2-propanol and water
  5. dry with materialThe wet O-desmethylvenlafaxine is dried in vacuo