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Ethanol → HCID 21293763、化合物

HRID 620814
ノート
印刷プレビュー

反応式

HRID 620814 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 86742939HCID 86742939、化合物

生成物 1

HCID 21293763HCID 21293763、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-a9a18e0372a74963a119d0465cf71098
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04822811

反応ノート

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