反応式
Cl.Cl.[F:3][C:4]([F:16])([F:15])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([CH2:13][NH2:14])[CH:8]=1.[C:17]([NH:20][C:21]1[CH:22]=[C:23]([CH:27]=[CH:28][N:29]=1)[C:24](O)=[O:25])(=[O:19])[CH3:18].C(N(CC)C(C)C)(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C)C=O.O>[C:17]([NH:20][C:21]1[CH:22]=[C:23]([CH:27]=[CH:28][N:29]=1)[C:24]([NH:14][CH2:13][C:9]1[CH:8]=[C:7]([O:6][CH2:5][C:4]([F:3])([F:15])[F:16])[CH:12]=[CH:11][N:10]=1)=[O:25])(=[O:19])[CH3:18]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
To a mixture of (4-(2,2,2-trifluoroethoxy)pyridin-2-yl)methanamine dihydrochloride (20 mg, 0.070 mmol, Amine-2), 2-acetamidoisonicotinic acid (15 mg, 0.084 mmol) and N,N-diisopropylethylamine (0.049 mL, 0.28 mmol) in N,N-dimethylformamide (0.5 mL) is added a solution of HBTU (40 mg, 0.11 mmol) in N,N-dimethylformamide (0.5 mL) at room temperature. After stirring at room temperature for 2 hours, the mixture is poured into water (2 mL) and extracted with ethyl acetate (3 mL). The organic layer is dried over sodium sulfate and concentrated under reduced pressure. The residue is purified by column chromatography on NH-silica gel eluting with ethyl acetate and then by preparative LC-MS to give 9.8 mg (38% yield) of the title compound.
後処理
- extractionextracted with ethyl acetate (3 mL)
- dry with materialThe organic layer is dried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue is purified by column chromatography on NH-silica gel eluting with ethyl acetate
出典と根拠
- ORDレコード
- ord-29829bd2666844e5b2e0022e1a8989de
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09302991B2
関連ノート
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