HRID1534471

反应详情

EQUATION

反应方程式

HRID 1534471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-butyryl-6-benzoyloxymethyl)-4(1H)-quinolone (30 g) was heated under reflux in phosphorus oxychloride (200 ml) for 30 minutes. The solvent was evaporated and the residue partitioned between dichloromethane and ammonia solution. The organic layer was washed successively with sodium hydrogen carbonate solution and 50% brine. Dried anhyd. MgSO4), filtered and evaporated to an oily solid which crystallized on trituration with petroleum ether to give 3-butyryl-4-chloro-6-benzyloxymethyl)quinoline (21.2 g, 67%), m.p. 85° C.-6° C.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. customthe residue partitioned between dichloromethane and ammonia solution
  3. washThe organic layer was washed successively with sodium hydrogen carbonate solution and 50% brine
  4. customDried
  5. filtrationMgSO4), filtered
  6. customevaporated to an oily solid which
  7. customcrystallized on trituration with petroleum ether