化工社化工社 化学情報印刷レポート · 研究参考用
Trifluoroacetic acid → 7-[5-(3,5-Dimethyl-isoxazol-4-ylmethyl)-2,5-diaza-bicyclo[2.2.1]hept-2-yl]-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isoxazole, 4-(chloromethyl)-3,5-dimethyl- | HCID 88246 | — |
| 反応物 | 7-(2,5-Diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine | HCID 68686236 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 7-[5-(3,5-Dimethyl-isoxazol-4-ylmethyl)-2,5-diaza-bicyclo[2.2.1]hept-2-yl]-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine | HCID 11177225 | — |
反応手順
The TFA salt of 7-(2,5-diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine (0.3 mmol; see Example 18 above) was dissolved in 3 mL of CH3CN along with 0.3 mmol of 4-chloromethyl-3,5-dimethyl-isoxazole (Aldrich-Sigma, St. Louis, Mo.) and 0.5 mmol of Et3N. The reaction mixture was stirred at room temperature for 18 hours. It was then concentrated and purified by preparative HPLC to afford the title compound. 1H NMR (400 Hz, DMSO-d6) δ 7.80 (d, J=1.0 Hz, 1H), 7.00 (d, J=3.6 Hz, 1H), 6.60 (dd, J=3.6, 1.0 Hz, 1H), 5.7 (s, 1H), 4.80 (brs, 2H), 2.4-3.6 (m, 14H). MS m/z: 407 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07834014B2 |
| 出典データセット | uspto-grants-2010_11 |
| ORD ID | ord-ff1540c77f164a4ebdad0305a39bbe0a |
| 出典メモ | uspto-grants-2010_11 |