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Dimethylformamide → N-[4-(4-Amino-pyrazolo[3,4-d]pyrimidin-1-yl)-phenyl]-4-methoxy-benzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Methoxybenzenesulfonyl chloride | HCID 7401 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-(4-Amino-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine | HCID 11995960 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-[4-(4-Amino-pyrazolo[3,4-d]pyrimidin-1-yl)-phenyl]-4-methoxy-benzenesulfonamide | HCID 11996549 | 70% |
反応手順
Title compound 11A, 1-(4-amino-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (36 mg, 1.1 eq, 0.16 mmol), 4-methoxybenzenesulphonylchloride (30 mg, 1.0 eq, 0.15 mmol) and diisopropylethylamine (25 μl, 1.0 eq, 0.15 mmol) were added to DMF (1 ml) and the mixture was stirred for 15 hours at room temperature under an inert atmosphere. Methanol was then added (1 ml) and the solvents were removed in vacuo. The resultant solid was purified by semi-preparative HPLC to yield the title compound as a white solid (40 mg, 0.10 mmol, 70%). LCMS: [M+H]+=397, Rt=1.66 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-49d20eba6391448b9c6dfd971f459b8a |
| 出典メモ | uspto-grants-2011_12 |