반응식
C[O-].[Na+].C([O:7][C@@H:8]1[CH2:12][N:11]([C:13](=[O:15])[CH3:14])[C@@H:10]([C:16]2[C:30]([O:31][C:32]3[CH:37]=[CH:36][C:35]([S:38]([CH3:41])(=[O:40])=[O:39])=[CH:34][CH:33]=3)=[CH:29][C:19]3[N:20]=[C:21]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=4)[NH:22][C:18]=3[CH:17]=2)[CH2:9]1)(=O)C>CO>[OH:7][C@@H:8]1[CH2:12][N:11]([C:13](=[O:15])[CH3:14])[C@@H:10]([C:16]2[C:30]([O:31][C:32]3[CH:33]=[CH:34][C:35]([S:38]([CH3:41])(=[O:39])=[O:40])=[CH:36][CH:37]=3)=[CH:29][C:19]3[N:20]=[C:21]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=4)[NH:22][C:18]=3[CH:17]=2)[CH2:9]1참가 물질
실험 절차
0.015 ml of 25% sodium methoxide was added to a methanol (2 ml) solution of 40 mg of trans-1-(4-acetoxy-2-(6-(4-methanesulfonyl-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone obtained in Example 325, and the reaction liquid was stirred at room temperature for 10 minutes. The solvent was evaporated away under reduced pressure, and the residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]. The solvent of the resulting fraction was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound as a white solid.
후처리
- customthe reaction liquid
- customThe solvent was evaporated away under reduced pressure
- customthe residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]
- additionThe solvent of the resulting fraction was diluted with ethyl acetate
- washwashed with aqueous saturated sodium bicarbonate
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated away under reduced pressure
출처 및 근거
- ORD 기록
- ord-47517cd23cb843e58edb72042e6fbf46
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07728025B2
연결된 노트
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