Formaldehyde → 2-(1-Acetylpiperidin-4-yl)propenal
반응식
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][OH:12])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Cl-].[CH3:14][NH2+]C.C=O>>[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([C:10](=[CH2:14])[CH:11]=[O:12])[CH2:8][CH2:9]1)(=[O:3])[CH3:2]참가 물질
4
실험 절차
3.95 g (23.3 mmol) of 2-(1-acetylpiperidin-4-yl)ethanol, 2.12 g (26.3 mmol) of dimethylammonium chloride and 3 ml (40 mmol) of 37% formaldehyde solution are heated at 110° C. for 2 hours with stirring. The mixture is allowed to cool and is extracted several times with diethyl ether. The organic phases are combined, washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated to dryness by evaporation. 2-(1-acetylpiperidin-4-yl)propenal is obtained in the form of a yellowish oil which can be further reacted without further purification.
후처리
- temperatureto cool
- extractionis extracted several times with diethyl ether
- washwashed with saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated to dryness by evaporation
출처 및 근거
- ORD 기록
- ord-22529da802a84b0abbec516a97fb4203
- 출처 데이터셋
- uspto-grants-1996_01
- 특허 번호
- US05488140
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