반응식
[CH3:1][N:2]([CH3:7])[S:3](Cl)(=[O:5])=[O:4].[F:8][C:9]([F:36])([F:35])[C:10]1[CH:19]=[C:18]2[C:13]([C:14]([NH:20][C:21]3[CH:34]=[CH:33][C:24]([C:25]([N:27]4[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]4)=[O:26])=[CH:23][CH:22]=3)=[CH:15][CH:16]=[N:17]2)=[CH:12][CH:11]=1.C(N(CC)CC)C>CN(C)C=O>[CH3:1][N:2]([CH3:7])[S:3]([N:30]1[CH2:31][CH2:32][N:27]([C:25](=[O:26])[C:24]2[CH:23]=[CH:22][C:21]([NH:20][C:14]3[C:13]4[C:18](=[CH:19][C:10]([C:9]([F:8])([F:35])[F:36])=[CH:11][CH:12]=4)[N:17]=[CH:16][CH:15]=3)=[CH:34][CH:33]=2)[CH2:28][CH2:29]1)(=[O:5])=[O:4]참가 물질
반응물 3
생성물 1
시약·촉매·용매 1
실험 절차
Dimethylsulfamoyl chloride (0.72 g, 0.54 ml, 0.005 mol) is added dropwise to a solution of 2.00 g (0.005 mol) of 4-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine and 2 ml of triethylamine in 20 ml of dimethylformamide. The reaction is stirred for 19 hours and then partitioned with chloroform-aqueous sodium carbonate. The organic phase is dried over anhydrous sodium sulfate, concentrated, and chromatographed with methylene chloride to 1% methanol/chloroform on silica gel to give 2.24 g of 1-[(dimethylamino)sulfonyl]-4-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine. This is crystallized from methylene chloride-cyclohexane to give 1.60 g of 1-[(dimethylamino)sulfonyl]-4-[4-[[-7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine of melting point 223°-224.5° C.
후처리
- custompartitioned with chloroform-aqueous sodium carbonate
- dry with materialThe organic phase is dried over anhydrous sodium sulfate
- concentrationconcentrated
- customchromatographed with methylene chloride to 1% methanol/chloroform on silica gel
출처 및 근거
- ORD 기록
- ord-99a38c6ca69b49cf937942d68aef5a69
- 출처 데이터셋
- uspto-grants-1979_09
- 특허 번호
- US04167567
연결된 노트
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