HRID1643289

反应详情

EQUATION

反应方程式

HRID 1643289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of NaH (605 mg, 60% oil dispersion) in 30 mL THF was slowly added at room temperature the crude (S)-6-(benzyloxy)-2-((R)-2-(4-fluorophenyl)-2-hydroxyethyl)hex-4-enoic acid isolated above as a solution in 5 mL THF. To this mixture was added dropwise methyl iodide (732 μL, 1.7 g, 11.3 mmol) and the resulting stirred for 3 h at room temperature. The reaction was quenched by the slow addition of 20 mL 1M aqueous HCl and the mixture extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine (2×30 mL) and dried over sodium sulfate. Evaporation of solvent afforded the product as an oil which was used directly in the next reaction without further purification.

WORKUP

后处理

  1. customThe reaction was quenched by the slow addition of 20 mL 1M aqueous HCl
  2. extractionthe mixture extracted with ethyl acetate (3×50 mL)
  3. washThe combined organic layers were washed with brine (2×30 mL)
  4. dry with materialdried over sodium sulfate
  5. customEvaporation of solvent