HRID1266950
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling the reaction mixture to room temperature
- filtrationthe solid was filtered
- customcollected
- dissolutionThe solid was then dissolved in methanol (50 ml)
- additioncharcoal (0.5 g) was added
- customThe charcoal was removed
- concentrationThe solution was then concentrated to a small volume
- customtriturated with ethyl acetate (100 ml)
- customThe solid was collected
- washwashed with ethyl acetate (2×30 ml)
- customdried in an oven under high vacuum at 50° C. overnight