HRID414232
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
1.5 g (10 mmol) of 2-chlorobenzaldehyde are boiled with 1.03 g (10 mmol) of nitroacetone, 2.7 g (20 mmol) of phenylacetone and 0.7 g (10 mmol) of ammonium acetate in 20 ml of ethanol overnight. The mixture is concentrated, the residue is taken up in ethyl acetate, and the solution is washed with water, dried and concentrated. The residue from evaporation is purified on a silica gel column using toluene/ethyl acetate 10:1. The fractions containing product are collected and concentrated. The substance crystallizes using ether. It is filtered off with suction and washed with ether. 200 mg of orange-colored crystals, of melting point 232° C., are obtained.
WORKUP
后处理
- concentrationThe mixture is concentrated
- washthe solution is washed with water
- customdried
- concentrationconcentrated
- customThe residue from evaporation
- customis purified on a silica gel column
- additionThe fractions containing product
- customare collected
- concentrationconcentrated
- customThe substance crystallizes
- filtrationIt is filtered off with suction
- washwashed with ether