참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Adenine | HCID 190 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 5-Chloro-2-chloromethyl-3-(2-fluorophenyl)-3H-quinazolin-4-one | HCID 22316557 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(6-Aminopurin-9-ylmethyl)-5-chloro-3-(2-fluorophenyl)-3H-quinazolin-4-one | HCID 10295762 | 50% |
반응 단계
Prepared according to Procedure C using Intermediate 2k (210 mg, 0.650 mmol), adenine (97 mg, 0.715 mmol), K2CO3 (99 mg, 0.715 mmol), and DMF (4 mL). The crude product was recrystallized from EtOH to provide 137 mg of a tan solid (50%), mp 295.6-295.8° C. (decomposes). 1H NMR (DMSO-d6) δ: 8.05 (s, 1H); 8.04 (s, 1H); 7.75 (t, J=7.6 Hz, 1H); 7.74 (t, J=7.9 Hz, 1H); 7.62-7.69 (m, 1H); 7.61 (d, J=7.6 Hz, 1H); 7.47-7.55 (m, 1H); 7.48 (d, J=7.8 Hz, 1H); 7.41 (d, J=8.0 Hz, 1H); 7.24 (br s, 2H); 5.19 (d, J=17 Hz, 1H); 5.03 (d, J=17 Hz, 1H). 13C NMR (DMSO-d6) ppm: 158.7, 157.6 (d, J=250 Hz), 156.2, 152.8, 152.4, 150.0, 149.2, 141.8, 135.4, 133.3, 132.5 (d, J=8.0 Hz), 131.0, 130.4, 127.3, 126.2 (d, J=3.5 Hz), 123.1 (d, J=14 Hz), 118.4, 117.6, 117.2 (d, J=19 Hz), 45.1. MS (ES): m/z 422.0 (M+). Anal. calcd. for C20H13ClFN7O.0.05C2H6O: C, 56.92; H, 3.16; Cl, 8.36; N, 23.12. Found: C, 56.79; H, 3.20; Cl, 8.46; N, 22.79.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06667300B2 |
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| 출처 데이터셋 | uspto-grants-2003_12 |
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| ORD ID | ord-188475ac640f4b8898fa02362e8c4139 |
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| 출처 메모 | uspto-grants-2003_12 |
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