HRID522877

反应详情

EQUATION

反应方程式

HRID 522877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a flask charged with tert-butyl 3-(1-hydroxyethyl)azetidine-1-carboxylate (212 mg, 1.053 mmol) was added THF (6.3 mL), resin bound PPh3 (527 mg, 1.580 mmol), p-chlorophenol (104 μL, 1.053 mmol) and DEAD (250 μL, 1.580 mmol). The reaction mixture was stirred overnight at RT. The reaction mixture was filtered through cotton and dried under reduced pressure, then purified with flash chromatography ramping CH2Cl2:MeOH:NH4OH (90:10:1) in CH2Cl2 from 0% to 100% to afford tert-butyl 3-(1-(4-chlorophenoxy)ethyl)-azetidine-1-carboxylate (145 mg, 44%) as a yellow oil.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through cotton
  2. customdried under reduced pressure
  3. custompurified with flash chromatography ramping CH2Cl2:MeOH:NH4OH (90:10:1) in CH2Cl2 from 0% to 100%