반응 #1379895

ord-175dfcd48372445b9432998d273d61af

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the layers were separated
  2. 2
    세척The organic solution was washed with diluted hydrochloric acid
  3. 3
    건조The organic layer was dried over magnesium sulfate
  4. 4
    여과filtered
  5. 5
    기타the solvent removed under reduced pressure
  6. 6
    기타The residue was purified by flash chromatography
  7. 7
    workup.ADDITIONa mixture of hexane and ethyl acetate
  8. 8
    기타The purification

실험 절차

A solution of acryloyl chloride dissolved in dry dichloromethane was cooled at 0° C. with an ice bath. A mixture of O-benzyl hydroxylamine hydrochloride (29) and N,N-diisopropylethylaamine in dry dichloromethane was added. Water was added and the layers were separated. The organic solution was washed with diluted hydrochloric acid, a saturated sodium bicarbonate solution, water, and brine. The organic layer was dried over magnesium sulfate, filtered, and the solvent removed under reduced pressure. The residue was purified by flash chromatography using a mixture of hexane and ethyl acetate. The purification gave N-benzyloxyacrylamide (30).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07238339B2uspto-grants-2007_07