HRID1720787

反应详情

EQUATION

反应方程式

HRID 1720787 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-4-thiaheptanoic acid p-methoxybenzyl ester as obtained in Reference Example 2 (1.99 g) in methylene chloride (26 ml), triethylamine (4.6 ml), palmitoyl chloride (6.00 g) and dimethylaminopyridine (5 mg) were added at 0° C., followed by stirring at room temperature for 24 hours. After addition of 5% citric acid, the reaction mixture was extracted with methylene chloride. The extract was washed with a saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and dried over anhydrous sodium sulfate, and the solvent was distilled off. The residue was recrystallized (methanol-hexane) to yield the title compound (2.30 g, yield 45%) as a white powder.

WORKUP

后处理

  1. additionwere added at 0° C.
  2. extractionthe reaction mixture was extracted with methylene chloride
  3. washThe extract was washed with a saturated aqueous solution of sodium hydrogen carbonate and saturated saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. customThe residue was recrystallized (methanol-hexane)