반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][OH:9])=[N:6][CH:7]=1.C(N(CC)CC)C.CS(Cl)(=O)=O.C(=O)([O-])[O-].[K+].[K+].[F:28][C:29]1[CH:41]=[C:40](O)[C:39]([F:43])=[CH:38][C:30]=1[C:31]([NH:33][S:34]([CH3:37])(=[O:36])=[O:35])=[O:32]>ClCCl.CS(C)=O.O>[CH2:5]([NH:6][CH2:7][CH3:2])[CH3:4].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][O:9][C:40]2[C:39]([F:43])=[CH:38][C:30]([C:31]([NH:33][S:34]([CH3:37])(=[O:36])=[O:35])=[O:32])=[C:29]([F:28])[CH:41]=2)=[N:6][CH:7]=1참가 물질
반응물 5
생성물 1
시약·촉매·용매 3
실험 절차
To a solution of (5-chloropyridin-2-yl)methanol (15 mg, 0.105 mmol), in dichloromethane (5 mL) and triethylamine (0.02 mL, 0.157 mmol) was added methanesulfonyl chloride (0.01 mL, 0.115 mmol). The reaction was stirred at room temperature for 2 hours. The solvent was removed in vacuo to afford a residue, which was taken up in DMSO (5 mL). Potassium carbonate (43 mg, 0.315 mmol) was added, followed by 2,5-difluoro-4-hydroxy-N-(methylsulfonyl)benzamide (Preparation 110, 29 mg, 0.115 mmol) and the reaction was heated to 50° C. overnight. The reaction mixture was cooled to room temperature, diluted with water (10 mL) and extracted with ethyl acetate (3×10 mL). The combined organic layers were dried over sodium sulphate, filtered and concentrated in vacuo. The resulting residue was purified by preparative HPLC to afford the title compound.
후처리
- customThe solvent was removed in vacuo
- customto afford a residue, which
- temperaturethe reaction was heated to 50° C. overnight
- temperatureThe reaction mixture was cooled to room temperature
- extractionextracted with ethyl acetate (3×10 mL)
- dry with materialThe combined organic layers were dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe resulting residue was purified by preparative HPLC
출처 및 근거
- ORD 기록
- ord-3f891cc096084a35aafa378cfe49e8d8
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09102621B2
연결된 노트
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