HRID454237

反应详情

EQUATION

反应方程式

HRID 454237 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of 7-(3-bromopropoxy)-6-methoxy-3-((pivaloyloxy)methyl) -3,4-dihydroquinazolin-4-one (36.7 g, 86 mmol) in 1-methylpiperazine (370 ml) was stirred at 100° C. for 90 minutes. After removal of the volatiles under vacuum, the residue was partitioned between methylene chloride and aqueous ammonium chloride. The organic layer was separated, washed with water, brine, dried (MgSO4) and evaporated. The solid was triturated with ether, filtered, washed with ether and dried under vacuum to give 7-(3-(4-methylpiperazin-1-yl)propoxy)-6-methoxy-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one (31.9 gr, 83%).

WORKUP

后处理

  1. customAfter removal of the volatiles under vacuum
  2. customthe residue was partitioned between methylene chloride and aqueous ammonium chloride
  3. customThe organic layer was separated
  4. washwashed with water, brine
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe solid was triturated with ether
  8. filtrationfiltered
  9. washwashed with ether
  10. customdried under vacuum