HRID637687
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 mixture of 14.2 g (82 mmole) of 4-chloro-3-nitrophenol, 12.4 g (90 mmole) of ground potassium carbonate, 8.2 g (55 mmole) of sodium iodide, 8.3 g (90 mmole) of chloroacetone and 220 ml of dimethylformamide is stirred for 3 hours at room temperature. The whole is subsequently filtered, the residue is washed with dimethylformamide, the organic phase is concentrated by evaporation in vacuo and the resulting crude product is partitioned between water and methylene chloride. The solid remaining after drying and removal of the methylene chloride is recrystallised from methylene chloride/petroleum ether. 1-(4-chloro-3-nitrophenoxy)-2-propanone is obtained having a melting point of 92°-94°.
WORKUP
后处理
- filtrationThe whole is subsequently filtered
- washthe residue is washed with dimethylformamide
- concentrationthe organic phase is concentrated by evaporation in vacuo
- customthe resulting crude product is partitioned between water and methylene chloride
- customafter drying
- customremoval of the methylene chloride
- customis recrystallised from methylene chloride/petroleum ether