HRID454095

反应详情

EQUATION

反应方程式

HRID 454095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 7-benzyloxy-4-(indol-5-yloxy)-6-methoxyquinazoline (8 g, 20 mmol) in DMF (50 ml) and methylene chloride (100 ml) containing 10% palladium on charcoal (2g) was hydrogenated at 1.8 atmospheres pressure until uptake of hydrogen had ceased. The solution was filtered, the catalyst was washed with DMF and the filtrate was evaporated. The residue was purified by column chromatography eluting with methylene chloride, followed by methylene chloride/methanol (95/5 and 90/10). After evaporation of the solvent, the residue was triturated with ether, filtered and dried under vacuum to give 7-hydroxy-4-(indol-5-yloxy)-6-methoxyquinazoline (2.7 g; 44%).

WORKUP

后处理

  1. filtrationThe solution was filtered
  2. washthe catalyst was washed with DMF
  3. customthe filtrate was evaporated
  4. customThe residue was purified by column chromatography
  5. washeluting with methylene chloride
  6. customAfter evaporation of the solvent
  7. customthe residue was triturated with ether
  8. filtrationfiltered
  9. customdried under vacuum