HRID4675

反应详情

EQUATION

反应方程式

HRID 4675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-acetyl-1-(3-nitrobenzyliden)acetone (10 g), benzamidine hydrochloride (8.06 g) and triethylamine (8.4 ml) in n-butanol (100 ml) was refluxed for 2 hours. The reaction mixture was added ethyl acetate (100 ml), washed with water (100 ml) and 5% hydrochloric acid (100 ml) successively. The solvent was evaporated and the residue was stirred with ethyl acetate (100 ml) for 1 hour. The crystals were collected by filtration, added a mixture of chloroform (100 ml) and water (100 ml) and adjusted to pH 8.5 by saturated potassium carbonate. The organic layer was evaporated in vacuo to give 5-acetyl-4-methyl-6-(3-nitrophenyl)-2-phenyl-1,6-dihydropyrimidine (4.46 g).

WORKUP

后处理

  1. temperaturewas refluxed for 2 hours
  2. washwashed with water (100 ml) and 5% hydrochloric acid (100 ml) successively
  3. customThe solvent was evaporated
  4. filtrationThe crystals were collected by filtration
  5. additionadded
  6. additiona mixture of chloroform (100 ml) and water (100 ml)
  7. customThe organic layer was evaporated in vacuo