HRID1768852
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
A mixture of 450 mg (1.38 mmole) of (3R, 5S)-5-[(1S)-1-(t-butoxycarbonyl)amino-2-cyclohexylethyl]-3-methyldihydrofuran-2(3H)-one (prepared as described in Preparation 2) and 10 ml of hexylamine was heated under reflux for 2.2 hours, whilst stirring. At the end of this time, the reaction mixture was concentrated by distillation under reduced pressure, after which the residue was purified by column chromatography through silica gel (using a 1:2 by volume mixture of cyclohexane and ethyl acetate as the eluent) to afford 443 mg of the title compound as white crystals.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 2.2 hours
- concentrationAt the end of this time, the reaction mixture was concentrated by distillation under reduced pressure
- customafter which the residue was purified by column chromatography through silica gel (
- additionby volume mixture of cyclohexane and ethyl acetate as the eluent)