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Butyric Acid → [4-(4-Amino-pyrazolo[3,4-d]pyrimidin-1-yl)-phenyl]-butyramide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butyric Acid | HCID 264 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 1-(4-Amino-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine | HCID 11995960 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [4-(4-Amino-pyrazolo[3,4-d]pyrimidin-1-yl)-phenyl]-butyramide | HCID 131729304 | 19.3% |
反応手順
Title compound 11A, 1-(4-amino-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (38 mg, 1.1 eq, 0.17 mmol) was added to a solution of butyric acid (13 mg, 1.0 eq, 0.15 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (26 mg, 1.1 eq, 0.17 mmol), 1-hydroxybenzotriazole (21 mg, 1.0 eq, 0.15 mmol) in DMF (1 ml) which had been stirred for 10 minutes under an inert atmosphere. The reaction was stirred at room temperature for 18 hours, after which methanol (1 ml) was added and the solvents were removed in vacuo. The resultant solid purified by semi-preparative HPLC to yield the title compound as a white solid (8.5 mg, 0.029 mmol, 19%). LCMS: [M+H]+=297, Rt=1.45 min, 100% purity.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08071607B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-dafc2ac356984b20b9b2bb4c5534eee8 |
| 出典メモ | uspto-grants-2011_12 |