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Diisopropylethylamine → 2-acetamido-N-((4-(2,2,2-trifluoroethoxy)pyridin-2-yl)methyl)isonicotinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 反応物 | 2-Acetamidopyridine-4-carboxylic acid | HCID 3774466 | — |
| 反応物 | (4-(2,2,2-Trifluoroethoxy)pyridin-2-yl)methanamine dihydrochloride | HCID 67510820 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-acetamido-N-((4-(2,2,2-trifluoroethoxy)pyridin-2-yl)methyl)isonicotinamide | HCID 56966008 | 38% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09302991B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-29829bd2666844e5b2e0022e1a8989de |
| 出典メモ | uspto-grants-2016_04 |