반응식
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]=[CH:13][C:12]([NH2:15])=[CH:11][N:10]=2)[CH:6]=[CH:7][CH:8]=1.[N+:18]([C:21]1[CH:29]=[CH:28][C:27]([N:30]2[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]2)=[CH:26][C:22]=1[C:23](O)=[O:24])([O-:20])=[O:19].CCN=C=NCCCN(C)C.Cl>ClCCl.CN(C)C1C=CN=CC=1.O>[N+:18]([C:21]1[CH:29]=[CH:28][C:27]([N:30]2[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]2)=[CH:26][C:22]=1[C:23]([NH:15][C:12]1[CH:13]=[N:14][C:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:16])[F:17])[CH:4]=2)=[N:10][CH:11]=1)=[O:24])([O-:20])=[O:19]참가 물질
7
반응물 3
생성물 1
시약·촉매·용매 3
실험 절차
To 2-(3-(trifluoromethyl)phenyl)pyrimidin-5-amine (750 mg, 3.14 mmol, 1.00 equiv) in dichloromethane (50 mL) was added 2-nitro-5-(piperidin-1-yl)benzoic acid (1.18 g, 4.72 mmol, 1.50 equiv), EDC.HCl (1.2 g, 6.28 mmol, 2.00 equiv) and 4-dimethylaminopyridine (770 mg, 6.31 mmol, 2.00 equiv) and the resulting solution was stirred for 48 h at room temperature. The reaction was diluted with 25 mL of water and then extracted with 2×25 mL of dichloromethane. The organic layers were combined, dried over sodium sulfate, concentrated, and the residue was applied onto a silica gel column and eluted with ethyl acetate/petroleum ether (1:30˜1:5) to give 0.4 g (27%) of product as a yellow solid.
후처리
- extractionextracted with 2×25 mL of dichloromethane
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- washeluted with ethyl acetate/petroleum ether (1:30˜1:5)
출처 및 근거
- ORD 기록
- ord-fda4d92259df47ecbe3978c8de8f0259
- 출처 데이터셋
- uspto-grants-2016_03
- 특허 번호
- US09289429B2
연결된 노트
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