HRID1099371
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
CONDITIONS
反应条件
- 温度
- 62.5 °C
PROCEDURE
实验过程
To a suspension of 4-Hydroxy-5-methyl-indan-1-one (50.0 gm, 0.308 mole) and Potassium carbonate (127.0 gm, 0.928 mole) in Dimethylformamide (250 ml), Dimethyl sulphate (90 ml, 0.928 mole) was added at 0° C. The reaction mixture was heated at 60-65° C. and stirred for 16 hours. The reaction mixture was poured into water (1 liter) and extracted with Ethylacetate (3×250 ml). The organic layer was dried over Sodium sulphate and distilled under vacuum to give 10.0 gm of crude product which was purified by column chromatography using Hexane as a mobile phase. The collected fractions were distilled under vacuum to give 45.0 gm of desired product as a viscous oil.
WORKUP
后处理
- additionwas added at 0° C
- extractionextracted with Ethylacetate (3×250 ml)
- dry with materialThe organic layer was dried over Sodium sulphate
- distillationdistilled under vacuum
- customto give 10.0 gm of crude product which
- customwas purified by column chromatography
- distillationThe collected fractions were distilled under vacuum