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 mixture of crude 2-acetoxy-1-(4(S)-benzyl-2,2-dimethyl-oxazolidin-3-yl)-2-[1-(biphenyl-4-yl)-1H-pyrrol-3-yl]-ethanone (1.82 mmol) and 10% palladium on carbon (120 mg) in EtOAc (4.5 mL) and EtOH (4.5 mL) was added ammonium formate (0.58 g, 9.2 mmol). After 40 hours at ambient temperature, the resultant mixture was filtered and the filtrate concentrated to a residue which was dissolved in EtOAc, washed with 1M pH7 phosphate buffer, dried over Na2SO4, and evaporated under reduced pressure to give a crude product. Flash column chromatography with 0-4% EtOAc/CH2Cl2 gradient eluant yielded 220 mg (43%) of 1-(4(S)-benzyl-2,2-dimethyl-oxazolidin-3-yl)-2-[1-(biphenyl-4-yl)-1H-pyrrol-3-yl]-ethanone as a pale yellow amorphous solid.
WORKUP
后处理
- filtrationthe resultant mixture was filtered
- concentrationthe filtrate concentrated to a residue which
- dissolutionwas dissolved in EtOAc
- washwashed with 1M pH7 phosphate buffer
- dry with materialdried over Na2SO4
- customevaporated under reduced pressure
- customto give a crude product