HRID2061358

反应详情

EQUATION

反应方程式

HRID 2061358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Compound 29 (450 mg, 2.56 mmol) was dissolved in EtOH (10 mL). NaBH4 (104 mg, 2.81 mmol) was added portionwise at 0° C., with vigorous stirring. The suspension was stirred at 0° C. for 15 min and then at room temperature for 1.5 h. Solvent was evaporated off in-vacuo. The resulting crude alcohol residue was dissolved in toluene (5 mL) and the solution was cooled to 0° C. PBr3 (240 μL, 2.56 mmol) was added dropwise over 10 min.

WORKUP

后处理

  1. waitat room temperature for 1.5 h
  2. customSolvent was evaporated off in-vacuo
  3. dissolutionThe resulting crude alcohol residue was dissolved in toluene (5 mL)
  4. temperaturethe solution was cooled to 0° C