HRID2092321
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
4-bromo-5-methylthiophene-2-carbaldehyde (11.00 g, 53 6 mmol) was treated with 2,2-dimethoxyethanamine (17.5 ml, 161 mmol) and the mixture stirred at 120° C. for 12 hours. The reaction was poured into water (50 ml) and stirred for 1 hour and extracted with ethyl acetate. The organic layer was washed (2×) with an aqueous saturated solution of sodium bicarbonate, then with water and then brine. The organic layer was then dried with sodium sulfate, concentrated under reduced pressure and placed under a vacuum line to give (E)-N-((4-bromo-5-methylthiophen-2-yl)methylene)-2,2-dimethoxyethanamine.
WORKUP
后处理
- stirringstirred for 1 hour
- extractionextracted with ethyl acetate
- washThe organic layer was washed (2×) with an aqueous saturated solution of sodium bicarbonate
- dry with materialThe organic layer was then dried with sodium sulfate
- concentrationconcentrated under reduced pressure