HRID1845132

反应详情

EQUATION

反应方程式

HRID 1845132 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)-2-(tert-butyldimethylsilyloxy)-1-(6-methylpyridin-3-yl)ethanol (15.6 g, 0.055 mol) and diphenylphosphonic azide (62.8 mL, 0.292 mol) in toluene (200 mL) at 0° C. was added 1,8-diazabicyclo[5.4.0]undec-7-ene (44.5 mL, 0.292 mol). The mixture was stirred at 0° C. for 30 minutes and then heated at 60° C. overnight. After cooling, the mixture was washed with water. The organic layer was dried and concentrated in vacuo. The residue was purified by flash chromatography (0-15% EtOAc/hexane) to afford a colorless oil.

WORKUP

后处理

  1. temperatureheated at 60° C. overnight
  2. temperatureAfter cooling
  3. washthe mixture was washed with water
  4. customThe organic layer was dried
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash chromatography (0-15% EtOAc/hexane)
  7. customto afford a colorless oil