2-Phenylacetophenone → 1,2-Diphenyl-1-ethanone oxime

HRID 975248

반응식

HRID 975248 반응식
[C:1]1([C:7](=O)[CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[OH:17][NH3+:18]>C(O)C>[C:1]1([C:7](=[N:18][OH:17])[CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 99482-PhenylacetophenoneHCID 21645Hydroxylamine HCl

생성물 1

HCID 2353831,2-Diphenyl-1-ethanone oxime수율 24.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1,2-diphenylethanone (19.6 g, 100 mmol) and hydroxyl ammonium chloride (13.9 g, 200 mmol) in absolute ethanol (200 ml) was heated at reflux for 4 h. The solvent was evaporated in vacuo and the residue extracted with dichloromethane (2×100 ml). The combined organic phases were washed with water (2×50 ml) and brine (10 ml) and dried (MgSO4). The solvent was evaporated in vacuo and the residue left for crystallisation. The crystallised product was suspended in n-heptane/diethylether 20/1 and the precipitate collected to give 5.1 g of 1,2-diphenylethanone oxime.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 4 h
  3. customThe solvent was evaporated in vacuo
  4. extractionthe residue extracted with dichloromethane (2×100 ml)
  5. washThe combined organic phases were washed with water (2×50 ml) and brine (10 ml)
  6. dry with materialdried (MgSO4)
  7. customThe solvent was evaporated in vacuo
  8. waitthe residue left for crystallisation
  9. customthe precipitate collected

출처 및 근거

ORD 기록
ord-69a8bb01e6504f2d91a4693128fd2ea4
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05608069

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