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
PROCEDURE
实验过程
A solution of 59.2 g (0.47 mole) of dimethyl sulphate and 32 g (0.517 mole) of dimethyl sulphide in 270 ml of acetonitrile is allowed to stir at room temperature for 5 days. Then, at 20° to 25° C., a solution of 87 g of 4-chlorophenyl 2-(p-chlorophenoxy)-2-propyl ketone in 80 ml of acetonitrile is added dropwise within about 2 hours. At the same temperature, 28.7 g (0.53 mole) of sodium methylate are added, the mixture is allowed to stir for 12 hours and then evaporated. The residue is vigorously stirred with a mixture of 200 ml of ethyl acetate and 150 ml of water overnight. The organic phase is separated off, dried over sodium sulphate and evaporated in vacuo. 49 g (76% of theory) of crude 2-(4-chlorophenyl)-2-[2-(p-chlorophenoxy)-2-propyl]oxirane are obtained, and this is immediately reacted further. ##STR47##
WORKUP
后处理
- stirringto stir for 12 hours
- customevaporated
- stirringThe residue is vigorously stirred with a mixture of 200 ml of ethyl acetate and 150 ml of water overnight
- customThe organic phase is separated off
- dry with materialdried over sodium sulphate
- customevaporated in vacuo