HRID1596259

反应详情

EQUATION

反应方程式

HRID 1596259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A mixture of 4-(3-acetoxy-4-methylanilino)-7-benzyloxy-6-methoxyquinazoline (2.68 g, 5.75 mmol) and 10% palladium-on-charcoal catalyst (0.27 g) in methanol (50 ml), DMF (12 ml) and trichloromethane (50 ml) was stirred at ambient temperature under hydrogen at 1.5 atmospheres pressure for 30 minutes. The catalyst was removed by filtration through diatomaceous earth and the solvent removed from filtrate by evaporation. The residue was triturated with ether, collected by filtration and dried under vacuum at 50° C. to give 4-(3-acetoxy-4-methylanilino)-7-hydroxy-6-methoxyquinazoline (2.1 g, 100%).

WORKUP

后处理

  1. customThe catalyst was removed by filtration through diatomaceous earth
  2. customthe solvent removed from filtrate by evaporation
  3. customThe residue was triturated with ether
  4. filtrationcollected by filtration
  5. customdried under vacuum at 50° C.