HRID2243291

反应详情

EQUATION

反应方程式

HRID 2243291 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

13.58 g (90.07 mmol) of t-butyidimethylsilyl chloride (TBDMSCl) were added to a solution of 10.00 g (81.89 mmol) of salicylaldehyde and 6.13 g (90.07 mmol) of imidazole in 82 ml of DMF. The mixture was stirred at room temperature and the reaction was monitored by thin-layer chromatography (cyclohexane/EA 10:1). 1 N NaOH was added, and the mixture was extracted with petroleum ether. The combined organic phases were dried over Na2SO4, the solvent was removed and the product was purified chromatographically (silica gel, cyclohexane/EA 10:1). This gave 16.94 g (87.5%) of a clear liquid.

WORKUP

后处理

  1. extractionthe mixture was extracted with petroleum ether
  2. dry with materialThe combined organic phases were dried over Na2SO4
  3. customthe solvent was removed
  4. customthe product was purified chromatographically (silica gel, cyclohexane/EA 10:1)