HRID1199697

反应详情

EQUATION

反应方程式

HRID 1199697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 25 g of 3-hydroxybenzaldehyde, 36.6 g of 2-methylbenzothiazole, 38.8 ml of acetic anhydride and 7.7 ml of formic acid was heated at 120° C. for 25 hours. The low boiling materials were evaporated together with toluene under reduced pressure, and the residue was added to 150 ml of methanol and refluxed with addition of 3 g of potassium carbonate for 1 hour. After cooled to room temperature, the mixture was filtered and filtrate was concentrated. The crude product formed was washed with methanol and ethyl ether and dried under reduced pressure to obtain 20.6 g (yield 40%) of the title compound.

WORKUP

后处理

  1. customThe low boiling materials were evaporated together with toluene under reduced pressure
  2. additionthe residue was added to 150 ml of methanol
  3. temperaturerefluxed with addition of 3 g of potassium carbonate for 1 hour
  4. temperatureAfter cooled to room temperature
  5. filtrationthe mixture was filtered
  6. concentrationfiltrate was concentrated
  7. customThe crude product formed
  8. washwas washed with methanol and ethyl ether
  9. customdried under reduced pressure