HRID622688

反应详情

EQUATION

反应方程式

HRID 622688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Iodomethane (6.9 ml) was added to a stirred suspension of 6-fluoro-4-hydroxyquinoline (16.3 g) and anhydrous potassium carbonate (15.2 g) in dry tetrahydrofuran (100 ml) at ambient temperature and stirring was continued for 18 hours. More iodomethane (1.8 ml) and anhydrous potassium carbonate (3.8 g) were added and stirring was continued for 4 hours at ambient temperature. Concentrated aqueous ammonia (specific gravity 0.88; 100 ml) was added and the mixture was evaporated to dryness. The residue was treated with water (200 ml) and extracted with dichloromethane (2×400 ml). The extract was dried and evaporated to dryness. The residue was crystallised from ethyl acetate to give the novel compound 6-fluoro-1-methyl-4-quinolone, m.p. 88°-89°.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 4 hours at ambient temperature
  3. customthe mixture was evaporated to dryness
  4. additionThe residue was treated with water (200 ml)
  5. extractionextracted with dichloromethane (2×400 ml)
  6. customThe extract was dried
  7. customevaporated to dryness
  8. customThe residue was crystallised from ethyl acetate