HRID358669

反应详情

EQUATION

反应方程式

HRID 358669 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-hydroxyquinol-3-yl methanesulphonate (0.48 g) and potassium carbonate (0.28 g) in dry dimethylformamide (20 ml) was stirred for 2 hours at ambient temperature. Methyl iodide (0.15 ml) was then added and the stirring at ambient temperature continued overnight. The solvent was removed under reduced pressure and the residue was triturated with water (10 ml). The resultant mixture was extracted extracts were evaporated to dryness. The residue was purified by flash chromatography on a silica gel column eluted with dichloromethane:methanol (39:1) followed by crystallisation from industrial methylated spirit (10 ml) to give the novel compound ]-methyl-4-oxo-1,4-dihydroquinol-3-yl methanesulphonate, m.p. 206°-208°.

WORKUP

后处理

  1. waitthe stirring at ambient temperature continued overnight
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was triturated with water (10 ml)
  4. extractionThe resultant mixture was extracted extracts
  5. customwere evaporated to dryness
  6. customThe residue was purified by flash chromatography on a silica gel column
  7. washeluted with dichloromethane:methanol (39:1)
  8. customfollowed by crystallisation from industrial methylated spirit (10 ml)