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Ethanol → HCID 21293763, 화합물

HRID 620814
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HRID 620814 반응식
[C:1](=[N:16][OH:17])([C:3]1[CH:4]=[CH:5][C:6]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[O:8][C:7]=2[CH:15]=1)[CH3:2].[CH2:18]([OH:20])[CH3:19].Cl.NO>N1C=CC=CC=1>[OH:17][N:16]([CH:1]([C:3]1[CH:4]=[CH:5][C:6]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[O:8][C:7]=2[CH:15]=1)[CH3:2])[C:18](=[O:20])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 86742939HCID 86742939, 화합물

생성물 1

HCID 21293763HCID 21293763, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

3-Acetyldibenzofuran oxime. The crude ketone prepared as described in step a, was dissolved in pyridine (50 mL) and ethanol (50 mL) and hydroxylamine hydrochloride was added. The mixture was stirred overnight at ambient temperature. The reaction was concentrated and the residue was partitioned between ethyl acetate (300 mL) and 3N HCl. The ethyl acetate layer was dried (Na2SO4), filtered and concentrated in vacuo to give a crystalline residue. The crystals were rinsed with hexane, filtered and dried to give 12.3 g of the desired product, mp 132°-135°.

후처리

  1. concentrationThe reaction was concentrated
  2. customthe residue was partitioned between ethyl acetate (300 mL) and 3N HCl
  3. dry with materialThe ethyl acetate layer was dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give a crystalline residue
  7. washThe crystals were rinsed with hexane
  8. filtrationfiltered
  9. customdried

출처 및 근거

ORD 기록
ord-a9a18e0372a74963a119d0465cf71098
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04822811

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