반응식
C([O:4][C:5]1[CH:6]=[C:7]([CH3:11])[CH:8]=[CH:9][CH:10]=1)(=O)C.[Al+3].[Cl-].[Cl-].[Cl-].Cl.[CH3:17][CH2:18][O:19]CC>>[CH3:11][C:7]1[CH:8]=[CH:9][C:10]([C:18]([CH3:17])=[O:19])=[C:5]([OH:4])[CH:6]=1참가 물질
5
반응 조건
- 온도
- 165 °C
실험 절차
To 50 g (0.33 mol) of 3-acetoxytoluene from Step 1 was added AlCl3 (60 g, 0.45 mol) and the resulting mixture was heated at 165° C. for 20 min., then cooled at 0° C. and HCl 1N was carefully added followed by Et2O. The aqueous phase was extracted 5× with Et2O and the combined organic phase wash washed with brine, dried over MgSO4 and evaporated. The residue was distilled under vacuum to give 42.2 (84%.) of the title compound.
후처리
- temperaturecooled at 0° C.
- extractionThe aqueous phase was extracted 5× with Et2O
- washthe combined organic phase wash
- washwashed with brine
- dry with materialdried over MgSO4
- customevaporated
- distillationThe residue was distilled under vacuum
출처 및 근거
- ORD 기록
- ord-7036ebfca3a74fa49644eddaecc7d22b
- 출처 데이터셋
- uspto-grants-1996_06
- 특허 번호
- US05527827
연결된 노트
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