HRID2368152

反应详情

EQUATION

反应方程式

HRID 2368152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A solution of 4-(2-cyclopropylethoxy)-2-nitrobenzaldehyde (0.79 g), tert-butyl {(1S)-2-[(trans-4-azidocyclohexyl)oxy]-1-methylethyl}carbamate (1.0 g), triphenylphosphine (3.08 g) and triethyl phosphite (3.08 g) in toluene (10 mL) was refluxed for 3 hr. The reaction mixture was allowed to cool, and concentrated under reduced pressure. To the obtained residue was added triethyl phosphite (4.0 g), and the mixture was stirred at 160° C. for 4 hr. The reaction mixture was allowed to cool, and purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (1.2 g).

WORKUP

后处理

  1. temperatureto cool
  2. concentrationconcentrated under reduced pressure
  3. additionTo the obtained residue was added triethyl phosphite (4.0 g)
  4. temperatureto cool
  5. custompurified by silica gel chromatography (hexane/ethyl acetate)