HRID77398
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
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
- temperaturethe mixture heated
- temperatureunder reflux for 23 h
- additionwas added
- temperaturethe reaction heated
- temperatureunder reflux until complete by Ic/ms
- temperatureOn cooling the reaction
- filtrationwas filtered
- customthe filtrate evaporated to dryness