반응 #473917

ord-fcf115bd39044ce0ba1f52f96e809d2e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONon completion of the dropwise addition
  2. 2
    추출extracted with ethyl acetate
  3. 3
    건조the organic layer was dried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

실험 절차

A solution of 4-methyl-3-nitrobenzaldehyde (3.5 g) in tetrahydrofuran (50 mL) was added dropwise to a solution of hydroxylamine hydrochloride (3.0 g) and sodium acetate (4.0 g) in tetrahydrofuran (50 mL) and water (50 mL) under ice cooling, and, on completion of the dropwise addition, the mixture was stirred for one hour at room temperature. The reaction solution was diluted with water and then extracted with ethyl acetate, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain a crude product of 4-methyl-3-nitrobenzaldehyde oxime (3.5 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08372867B2uspto-grants-2013_02