HRID2307441
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 6-acetyl-3,4-dihydro-2H-quinoline-1-carboxylic acid tert-butyl ester (1.38 g, 5 mmol) in EtOH (20 mL) was treated with NH2OH.HCl (695 mg, 10 mmol). The resulting solution was stirred at 23° C. for 3 hours in the presence of Amberlist A-21 (2.0). Then the mixture was filtered and the solvent evaporated. The residue was dissolved in EtOAc, washed with aqueous NaHCO3 and then brine. After drying (MgSO4), the organic layer was concentrated and the crude oxime purified by chromatography (SiO2, 10-25% EtOAc in hexane) to give 1.4 g (90%) of the title compound as a white solid. m.p: 127-129° C.
WORKUP
后处理
- filtrationThen the mixture was filtered
- customthe solvent evaporated
- dissolutionThe residue was dissolved in EtOAc
- washwashed with aqueous NaHCO3
- dry with materialAfter drying (MgSO4)
- concentrationthe organic layer was concentrated
- customthe crude oxime purified by chromatography (SiO2, 10-25% EtOAc in hexane)