HRID1380860
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
N-chloroacetyl-N-[2-(3-methoxy-phenyl)-ethyl]amine (3.1 g, 0.0136 mol) is dissolved in ethanol (270 ml) and water (1530 ml) and illuminated for 10 hours in a nitrogen atmosphere at 20°-25° C. with a high pressure mercury lamp. The solution is evaporated down (about 400 ml), mixed with sodium bicarbonate and extracted several times with ethyl acetate. The extracts are dried over magnesium sulphate, concentrated by evaporation and the residue is purified over a silica gel column with ethyl acetate as eluant. Yield: 820 mg. Mp: 152°-154° C.
WORKUP
后处理
- customThe solution is evaporated down (about 400 ml)
- additionmixed with sodium bicarbonate
- extractionextracted several times with ethyl acetate
- dry with materialThe extracts are dried over magnesium sulphate
- concentrationconcentrated by evaporation
- customthe residue is purified over a silica gel column with ethyl acetate as eluant