HRID1720802

反应详情

EQUATION

反应方程式

HRID 1720802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 6,7-dihydroxy-2-methyl-4-thiaheptanoic acid t-butyl ester as obtained in Reference Example 40 (500 mg) in chloroform (30 ml), triethylamine (5.6 ml), palmitoyl chloride (5.50 g) and dimethylaminopyridine (5 mg) were added, followed by stirring at room temperature for 48 hours. After addition of water, the reaction mixture was extracted with ethyl acetate. The extract was washed with a 5% aqueous solution of citric acid, a saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and dried over anhydrous sodium sulfate, and the solvent was distilled off. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to yield the title compound (1.33 g, yield 91%) as a colorless oily substance.

WORKUP

后处理

  1. additionwere added
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. washThe extract was washed with a 5% aqueous solution of citric acid
  4. dry with materiala saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and dried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)