HRID1714434

反应详情

EQUATION

反应方程式

HRID 1714434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A mixture of 5-Hydroxy-6-indan-1-one, Intermediate H, (0.50 g, 0.0028 mol), 4-chloromethyl-2,2-dimethyl-1,3-dioxolane (0.766 mL, 0.0056 mol), potassium carbonate (1.54 g, 0.011 mol) and DMF (20.0 mL) was stirred at 95° C. for 3 days. Water (150.0 mL) was added and the mixture was extracted with ethyl acetate (2×150 mL). The organic layer was washed with sat. NaHCO3, brine and dried over Na2SO4. The solvent was then removed in vacuo to yield 5-(2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-6-methoxy-indan-1-one (Intermediate I) as light brown solid. MS m/z 293 (M+H)+.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate (2×150 mL)
  2. washThe organic layer was washed with sat. NaHCO3, brine
  3. dry with materialdried over Na2SO4
  4. customThe solvent was then removed in vacuo