HRID1845131

反应详情

EQUATION

反应方程式

HRID 1845131 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred mixture of (R)-1-(6-methylpyridin-3-yl)ethane-1,2-diol (13.72 g, 0.085 mol), 1H-imidazole (13.55 g, 0.197 mol), and CH2Cl2 (180 mL) at 0° C. was added tert-butyldimethylsilyl chloride (15.31 g, 0.098 mol). The reaction mixture was stirred at 0° C. for 30 minutes, then warmed to room temperature and stirred overnight. The mixture was washed with water (300 mL) and extracted with CH2Cl2. The combined organic layers were dried over sodium sulfate, and concentrated. The residue was purified by flash chromatography (0-50% EtOAc/hexane) to afford a colorless oil.

WORKUP

后处理

  1. temperaturewarmed to room temperature
  2. stirringstirred overnight
  3. washThe mixture was washed with water (300 mL)
  4. extractionextracted with CH2Cl2
  5. dry with materialThe combined organic layers were dried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by flash chromatography (0-50% EtOAc/hexane)
  8. customto afford a colorless oil