HRID129660

反应详情

EQUATION

反应方程式

HRID 129660 的结构方程式

CONDITIONS

反应条件

温度
-30 °C

PROCEDURE

实验过程

3.3 cm3 of thionyl chloride are added over 10 minutes to 30 cm3 of methanol cooled to a temperature in the region of -30° C. Stirring is maintained for 30 minutes at a temperature in the region of -23° C. and then 4.7 g of 4-aminomethylbenzoic acid are added. The mixture is left to return to a temperature in the region of 20° C. over 1 hour. The mixture is treated with 15 cm3 of methanol and stirring is maintained for 15 hours at a temperature in the region of 20° C. The solid is separated by filtration, rinsed with a total of 90 cm3 of methanol and then with a total of 150 cm3 of diethyl ether. The solid is dried under reduced pressure (13.5 Pa) at a temperature in the region of 20° C. 3.2 g of methyl 4-aminomethylbenzoate hydrochloride are thus obtained in the form of a white solid melting at a temperature in the region of 270° C.

WORKUP

后处理

  1. temperatureis maintained for 30 minutes at a temperature in the region of -23° C.
  2. waitThe mixture is left
  3. stirringstirring
  4. temperatureis maintained for 15 hours at a temperature in the region of 20° C
  5. customThe solid is separated by filtration
  6. washrinsed with a total of 90 cm3 of methanol
  7. customThe solid is dried under reduced pressure (13.5 Pa) at a temperature in the region of 20° C