HRID1978355

反应详情

EQUATION

反应方程式

HRID 1978355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Under nitrogen, 5.41 g (35.9 mM) of tert-butyldimethylsilyl chloride was added to a solution of 7.69 g (27.63 mM) of methyl 6-hydroxy-2,5,7,8-tetramethylchroman-2-acetate and 2.82 g (41.4 mM) of imidazole in DMF (54 ml) at room temperature and the mixture was stirred at 0° C. for 20 hours. This reaction mixture was poured in saturated aqueous sodium hydrogen carbonate-diethyl ether under intense agitation to stop the reaction and, then, extracted with diethyl ether. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over MgSO4. The resulting crude product was purified by column chromatography (ethyl acetate-hexane: 10%) to provide the title compound as yellow oil.

WORKUP

后处理

  1. customthe reaction
  2. extractionextracted with diethyl ether
  3. washThe organic layer was washed with water and saturated aqueous solution of sodium chloride
  4. dry with materialdried over MgSO4
  5. customThe resulting crude product was purified by column chromatography (ethyl acetate-hexane: 10%)