HRID1353978
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionextracted with ethyl acetate (200 ml×2) The organic layer
- washwas washed with water (100 ml×2)
- customevaporated
- stirringthe residue stirred with ammonium hydroxide (50 ml) for 2 hrs
- customto quench any unreacted dimethyl sulfate
- extractionProduct was extracted with ethyl acetate (200 ml)
- washwas washed with water (100 ml×2) and brine (100 ml)
- customThe solvent was evaporated