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2-Thiophenecarbonyl chloride → HCID 178522594、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Thiophenecarbonyl chloride | HCID 78928 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | HCID 178508735 | HCID 178508735 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | HCID 178522594 | HCID 178522594 | 12.7% |
反応手順
To a solution of N2-Benzyl-5-(1H-tetrazol-5-yl)pyrimidine-2,4-diamine (27 mg, 0.1 mmol) in 1 mL of DCE, DIPEA (0.3 mmol, 3.0 eq.) was added followed by thiophene-2-carbonyl chloride (0.15 mmol, 1.5 eq.). The reaction was stirred at room temperature for 2 hours. The crude reaction mixture was concentrated down in vacuo, and the residue redissolved in ethylacetate. This organic solution was extracted several times with water, dried with magnesium sulfate, filtered and concentrated. The residue was purified by reverse phase HPLC to give 4.8 mg of the desired compound. 1H-NMR (400 MHz, d6-DMSO): δ 9.07 (t, 1H), 7.81 (dd, 1H), 7.77 (dd, 1H), 7.36-7.29 (m, 4H), 7.28-7.23 (m, 1H), 7.16 (t, 1H), 4.45 (d, 2H). MS (EI) for C17H14N8OS: 379 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08053454B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-f24f64ac25344978a1204289b413d221 |
| 出典メモ | uspto-grants-2011_11 |