HRID2307441

反应详情

EQUATION

反应方程式

HRID 2307441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationThen the mixture was filtered
  2. customthe solvent evaporated
  3. dissolutionThe residue was dissolved in EtOAc
  4. washwashed with aqueous NaHCO3
  5. dry with materialAfter drying (MgSO4)
  6. concentrationthe organic layer was concentrated
  7. customthe crude oxime purified by chromatography (SiO2, 10-25% EtOAc in hexane)