HRID414232

反应详情

EQUATION

反应方程式

HRID 414232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe mixture is concentrated
  2. washthe solution is washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue from evaporation
  6. customis purified on a silica gel column
  7. additionThe fractions containing product
  8. customare collected
  9. concentrationconcentrated
  10. customThe substance crystallizes
  11. filtrationIt is filtered off with suction
  12. washwashed with ether