Diisopropylethylamine → 2-[(1-Methyl-1-{1-[2-(methylsulfonyl)-4-(trifluoromethoxy)benzoyl]piperidin-4-yl}ethyl)sulfonyl]-6-(trifluoromethyl)pyridine
반응식
[CH3:1][S:2]([C:5]1[CH:13]=[C:12]([O:14][C:15]([F:18])([F:17])[F:16])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=O)(=[O:4])=[O:3].[CH3:19][C:20]([S:28]([C:31]1[CH:36]=[CH:35][CH:34]=[C:33]([C:37]([F:40])([F:39])[F:38])[N:32]=1)(=[O:30])=[O:29])([CH:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)[CH3:21].CN([P+](ON1N=NC2C=CC=CC1=2)(N(C)C)N(C)C)C.F[P-](F)(F)(F)(F)F.C(N(C(C)C)CC)(C)C>CS(C)=O.O.FC(F)(F)C(O)=O.CN(C)C=O>[CH3:21][C:20]([S:28]([C:31]1[CH:36]=[CH:35][CH:34]=[C:33]([C:37]([F:39])([F:40])[F:38])[N:32]=1)(=[O:30])=[O:29])([CH:22]1[CH2:23][CH2:24][N:25]([C:7](=[O:9])[C:6]2[CH:10]=[CH:11][C:12]([O:14][C:15]([F:18])([F:17])[F:16])=[CH:13][C:5]=2[S:2]([CH3:1])(=[O:3])=[O:4])[CH2:26][CH2:27]1)[CH3:19]참가 물질
9
반응물 4
생성물 1
시약·촉매·용매 4
실험 절차
To a 10 ml vial was added 2-(methylsulfonyl)-4-(trifluoromethoxy)benzoic acid (16.9 mg, 0.059 mmol), 2-[(1-methyl-1-piperidin-4-ylethyl)sulfonyl]-6-(trifluoromethyl)pyridine (20 mg, 0.059 mmol), Bop reagent (31.6 mg, 0.071 mmol), diisopropylethyl amine (0.052 ml, 0.297 mmol) and 1 ml dimethylformamide. The resulting solution was stirred at room temperature for 1 hour. It was diluted with 1 m dimethyl sulfoxide, 0.5 ml water and 0.1 ml trifluoroacetic acid. This mixture was loaded on to reverse phase column directly and eluted with water acetonitrile gradient solvent to give the title compound as fluffy white solid after lyophilizing.
후처리
- washeluted with water acetonitrile gradient solvent
출처 및 근거
- ORD 기록
- ord-b8b50378c77a4b3195d3d8de95b36b44
- 출처 데이터셋
- uspto-grants-2012_11
- 특허 번호
- US08304434B2
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