HRID561477
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
- 0 °C
PROCEDURE
实验过程
1.50 g (10.67 mmol) of 4-chlorobenzaldehyde were dissolved in 20 ml of diethyl ether at 0° C., and 32.0 ml (16.00 mmol) of a 0.5N solution of cyclopropylmagnesium bromide in tetrahydrofuran were slowly added dropwise. Stirring at 0° C. for 1 h was followed by warming to RT, addition of water and ethyl acetate to the reaction solution, and separation of the phases. The organic phase was dried over sodium sulfate, the solid was filtered off, and the solvents were removed in vacuo. The crude product was purified by preparative HPLC (mobile phase: acetonitrile/water gradient) to result in 1.21 g (62% of theory) of the title compound.
WORKUP
后处理
- temperatureby warming to RT
- customto the reaction solution, and separation of the phases
- dry with materialThe organic phase was dried over sodium sulfate
- filtrationthe solid was filtered off
- customthe solvents were removed in vacuo
- customThe crude product was purified by preparative HPLC (mobile phase: acetonitrile/water gradient)