반응식
[Si]([O:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]1[CH:22]=[C:21]2[C:16]([CH:17]=[C:18]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]([F:33])([F:32])[F:31])[NH:19][C:20]2=[O:23])=[CH:15][CH:14]=1)(C(C)(C)C)(C)C.C(Cl)Cl>C1COCC1>[OH:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]1[CH:22]=[C:21]2[C:16]([CH:17]=[C:18]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]([F:33])([F:31])[F:32])[NH:19][C:20]2=[O:23])=[CH:15][CH:14]=1참가 물질
실험 절차
The 7-[3-(tert-butyldimethylsilyloxy)propylamino]-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (435 mg, 0.913 mmol) obtained in step A was dissolved in THF (9 ml). Thereafter, a 1 M tetrabutylammonium fluoride THF solution (1.1 ml, 1.1 mmol) was added to the obtained solution at a room temperature. The obtained mixture was stirred for 5 hours. Thereafter, methylene chloride was added to the reaction solution. An organic layer thereof was washed with a saturated saline solution, and was then dried over magnesium sulfate, followed by concentration under reduced pressure. The obtained residue was purified by silica gel chromatography (methylene chloride:methanol=30:1), so as to obtain 7-(3-hydroxypropylamino)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (337 mg, 95%).
후처리
- washAn organic layer thereof was washed with a saturated saline solution
- dry with materialwas then dried over magnesium sulfate
- concentrationfollowed by concentration under reduced pressure
- customThe obtained residue was purified by silica gel chromatography (methylene chloride:methanol=30:1)
출처 및 근거
- ORD 기록
- ord-1fa931e1f50d42229998f1077252e940
- 출처 데이터셋
- uspto-grants-2010_10
- 특허 번호
- US07820693B2
연결된 노트
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