HRID1845145

反应详情

EQUATION

反应方程式

HRID 1845145 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A round bottom flask was charged with 1-(4-chloro-3-(methylsulfonyl)phenyl)ethanol (8.5 g, 32.44 mmol) and toluene (100 mL). Diphenyl phosphoryl azide (8.4 mL, 38.93 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (5.8 mL, 38.93 mmol) were added at 0° C. and the mixture was stirred over night at room temperature. The volatiles were removed under reduced pressure and the residue was diluted with water and extracted with EtOAc. The combined organic layers were concentrated under reduced pressure and the residue was purified by column chromatography to get the product (2.4 g, 28% yield).

WORKUP

后处理

  1. customThe volatiles were removed under reduced pressure
  2. additionthe residue was diluted with water
  3. extractionextracted with EtOAc
  4. concentrationThe combined organic layers were concentrated under reduced pressure
  5. customthe residue was purified by column chromatography