HRID77398

反应详情

EQUATION

反应方程式

HRID 77398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-amino-5-hydroxy-N-methylbenzamide (Intermediate 32A) (280 mg, 1.68 mmol) and 3-chlorobenzaldehyde (0.23 mL, 2.02 mmol) in ethanol (10 mL) was added a catalytic amount of acetic acid (0.07 mL) and the mixture heated under reflux for 23 h. The reaction was cooled before manganese (iv) oxide (225 mg, 1.68 mmol) was added and the reaction heated under reflux until complete by Ic/ms. On cooling the reaction was filtered and the filtrate evaporated to dryness to afford 2-(3-chlorophenyl)-6-hydroxy-3-methylquinazolin-4(3H)-one (450 mg, 1.57 mmol).

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 23 h
  3. additionwas added
  4. temperaturethe reaction heated
  5. temperatureunder reflux until complete by Ic/ms
  6. temperatureOn cooling the reaction
  7. filtrationwas filtered
  8. customthe filtrate evaporated to dryness