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 methyl 3-[[5-[3-[[tert-butyl(dimethyl)silyl]oxymethyl]-1-piperidyl]-2-methyl-benzoyl]amino]-2,4-dimethyl-benzoate (0.60 g, 1.14 mmol) in THF (15 ml) is added Bu4NF 1.0 M in THF (0.596 g, 2.28 mmol) at 0° C. The reaction mixture is gradually warmed to ambient temperature. After 1 hour, the reaction mixture is diluted with ice-water and extracted with ethyl acetate. The organic layers are combined, dried over sodium sulfate, filtered, and concentrated under reduced pressure to give a residue. The residue is purified by flash chromatography (silica gel) over a gradient using 4% methanol in dichloromethane as eluent to afford the title compound as a white solid (0.4 g, 85.5%). Mass spectrum (m/z): 411.4 (M+1).
WORKUP
后处理
- extractionextracted with ethyl acetate
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto give a residue
- customThe residue is purified by flash chromatography (silica gel) over a gradient