HRID718666
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 solution of compound 58a (6.0 g, 17 mmol) in trifluoroacetic acid (20 mL) was hydrogenated at about 2 to 3 atm over PtO2 (0.4 g, 1.8 mmol) at 30° C. for 20 h. The resulting mixture was filtered through a pad of diatomaceous earth and the filtrate was concentrated under reduced pressure. The residue obtained was purified by flash column chromatography on silica gel (EtOAc/petroleum ether (1:2 v/v)) to obtain compound 58b as a colorless oil. Mass Spectrum (LCMS, ESI pos.): Calcd. for C28H27N5O3: 284.1 (M+H). Found: 284.2.
WORKUP
后处理
- filtrationThe resulting mixture was filtered through a pad of diatomaceous earth
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue obtained
- customwas purified by flash column chromatography on silica gel (EtOAc/petroleum ether (1:2 v/v))