HRID1266950

反应详情

EQUATION

反应方程式

HRID 1266950 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 solution of 6-methoxy-2-methylbenzothiazole (1.82 g) and 2-bromoethanol (8.8 g) was stirred and heated in an oil bath at 120° C. for 74 hours. After cooling the reaction mixture to room temperature, adding ethyl acetate (25 ml) and stirring for 1 hour, the solid was filtered and collected. The solid was then dissolved in methanol (50 ml) and charcoal (0.5 g) was added. The charcoal was removed by passing through a pad of Celite®. The solution was then concentrated to a small volume and triturated with ethyl acetate (100 ml). The solid was collected, washed with ethyl acetate (2×30 ml) and dried in an oven under high vacuum at 50° C. overnight to obtain 0.9 g (30%) of 4c.

WORKUP

后处理

  1. temperatureAfter cooling the reaction mixture to room temperature
  2. filtrationthe solid was filtered
  3. customcollected
  4. dissolutionThe solid was then dissolved in methanol (50 ml)
  5. additioncharcoal (0.5 g) was added
  6. customThe charcoal was removed
  7. concentrationThe solution was then concentrated to a small volume
  8. customtriturated with ethyl acetate (100 ml)
  9. customThe solid was collected
  10. washwashed with ethyl acetate (2×30 ml)
  11. customdried in an oven under high vacuum at 50° C. overnight