HRID324936

反应详情

EQUATION

反应方程式

HRID 324936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1,3-Dihydroxynaphthalene (15 g, 93.6 mmol) and potassium carbonate (20 g, 144.7 mmol) in acetone (200 ml) was added dimethyl sulfate (21 ml, 222 mmol). After stirring over-night the reaction mixture was mixed with 10% sodium hydroxide (100 ml) and extracted with ethyl acetate (200 ml×2) The organic layer was washed with water (100 ml×2), evaporated, and the residue stirred with ammonium hydroxide (50 ml) for 2 hrs to quench any unreacted dimethyl sulfate. Product was extracted with ethyl acetate (200 ml) and was washed with water (100 ml×2) and brine (100 ml). The solvent was evaporated yielding 15 g (85%) of 6.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (200 ml×2) The organic layer
  2. washwas washed with water (100 ml×2)
  3. customevaporated
  4. stirringthe residue stirred with ammonium hydroxide (50 ml) for 2 hrs
  5. customto quench any unreacted dimethyl sulfate
  6. extractionProduct was extracted with ethyl acetate (200 ml)
  7. washwas washed with water (100 ml×2) and brine (100 ml)
  8. customThe solvent was evaporated