HRID1099371

反应详情

EQUATION

反应方程式

HRID 1099371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added at 0° C
  2. extractionextracted with Ethylacetate (3×250 ml)
  3. dry with materialThe organic layer was dried over Sodium sulphate
  4. distillationdistilled under vacuum
  5. customto give 10.0 gm of crude product which
  6. customwas purified by column chromatography
  7. distillationThe collected fractions were distilled under vacuum