HRID2368151

反应详情

EQUATION

反应方程式

HRID 2368151 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl {(1S)-2-[(cis-4-hydroxycyclohexyl)oxy]-1-methylethyl}carbamate (5.00 g), triphenylphosphine (7.20 g) and diphenylphosphorylazide (5.03 g) in toluene (200 mL) was added dropwise a solution (1.9 M, 14.4 mL) of diisopropyl azodicarboxylate in toluene, and the mixture was stirred at room temperature for 16 hr. The reaction mixture was concentrated under reduced pressure, the residue was suspended in diethyl ether, and the precipitate was removed by filtration. The filtrate was concentrated, and the residue was purified by silica gel chromatography(hexane/ethyl acetate) to give the title compound (1.05 g).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe precipitate was removed by filtration
  3. concentrationThe filtrate was concentrated
  4. customthe residue was purified by silica gel chromatography(hexane/ethyl acetate)