반응식
CC1(C)[CH2:7][CH2:6][CH:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[CH2:4][CH2:3]1.[CH2:21](N(CC)CC)C.[C:28](Cl)(=[O:32])[CH2:29][CH2:30][CH3:31].C(=O)([O-])O.[Na+].O1[CH2:43][CH2:42][CH2:41][CH2:40]1>C(OCC)(=O)C>[CH2:41]([C:42]1([CH2:43][CH3:21])[CH2:7][CH2:6][CH:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N:14]2[CH2:15][CH2:16][N:17]([C:28](=[O:32])[CH2:29][CH2:30][CH3:31])[CH2:18][CH2:19]2)[CH2:4][CH2:3]1)[CH3:40]참가 물질
반응 조건
- 온도
- 0 °C
실험 절차
To a solution of 1-[2-(4,4-dimethylcyclohexyl)phenyl]piperazine (30 mg, 0.10 mmol) produced in Example (83a) in tetrahydrofuran (1 mL) was added triethylamine (15 mg, 0.15 mmol), followed by stirring at an external temperature of 0° C. Butyryl chloride (0.015 mL, 0.14 mmol) was added to the reaction mixture while stirring, and the stirring was continued for 9 hours and 30 minutes at an external temperature of 0° C. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The organic layer was washed with water and filtered through Celite, and the filtrate was concentrated. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 27 mg of the title compound as a yellow solid.
후처리
- stirringwhile stirring
- washThe organic layer was washed with water
- filtrationfiltered through Celite
- concentrationthe filtrate was concentrated
- customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane)
출처 및 근거
- ORD 기록
- ord-5fb9d8f480d444178b075c450a11506a
- 출처 데이터셋
- uspto-grants-2008_08
- 특허 번호
- US07410971B2
연결된 노트
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