関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Adenine | HCID 190 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-Chloro-2-chloromethyl-3-(2-chlorophenyl)-3H-quinazolin-4-one | HCID 22316565 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(6-Aminopurin-9-ylmethyl)-6-chloro-3-(2-chlorophenyl)-3H-quinazolin-4-one | HCID 10181599 | 39% |
反応手順
Prepared according to Procedure C using Intermediate 2d (100 mg, 0.294 mmol), adenine (44 mg, 0.323 mmol), K2CO3 (45 mg, 0.323 mmol), and DMF (1 mL). The crude product was recrystallized from EtOH to provide 50 mg of a yellow solid (39%), mp 294.5-294.8° C. (decomposes). 1H NMR (DMSO-d6) δ: 8.10 (d, J=2.2 Hz, 1H); 8.05 (s, 1H); 8.03 (s, 1H); 7.86 (dd, J=2.4, 8.8 Hz, 1H); 7.75-7.82 (m, 2H); 7.59-7.67 (m, 2H); 7.53 (d, J=8.7 Hz, 1H); 7.22 (br s, 2H); 5.13 (d, J=17 Hz, 1H); 4.95 (d, J=17 Hz, 1H). 13C NMR (DMSO-d6) ppm: 159.7, 156.2, 152.9, 151.9, 150.1, 145.5, 141.8, 135.7, 133.1, 132.3, 132.2, 131.9, 131.1, 130.9, 130.0, 129.4, 125.9, 122.0, 118.4, 44.9. MS (ES): m/z 438.0 (M+). Anal. calcd. for C20H13Cl2N7O: C, 54.81; H, 2.99; N, 22.37. Found: C, 54.72; H, 2.87; N, 22.18.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653077B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-9c0b3e0db9794f86be9d023ebc14ab4d |
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| 出典メモ | uspto-grants-2014_02 |
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