HRID2368151
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe precipitate was removed by filtration
- concentrationThe filtrate was concentrated
- customthe residue was purified by silica gel chromatography(hexane/ethyl acetate)