참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Chloromethyl-3-(2-chlorophenyl)-5-methyl-3H-quinazolin-4-one | HCID 22316547 | — |
| 반응물 | HCID 178527204 | HCID 178527204 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178423980 | HCID 178423980 | 79.3% |
반응 단계
Prepared according to Procedure C using Intermediate 2g (300 mg, 0.940 mmol), 6-mercaptopurine monohydrate (176 mg, 1.03 mmol), K2CO3 (142 mg, 1.03 mmol), and DMF (5 mL). The crude product was recrystallized from EtOH to provide 324 mg of a white crystalline solid (79%), mp 227.8-230.1° C. (decomposes). 1H NMR (DMSO-d6) δ: 13.57 (br s, 1H); 8.49 (s, 1H); 8.47 (s, 1H); 7.69-7.78 (m, 2H); 7.66 (d, J=7.3 Hz, 1H); 7.55 (d, J=7.9 Hz, 1H); 7.39-7.52 (m, 2H); 7.36 (d, J=6.9 Hz, 1H); 4.38-4.50 (m, 2H); 2.74 (s, 3H). 13C NMR (DMSO-d6) ppm: 161.2, 156.3, 152.4, 151.5, 148.6, 143.9, 141.0, 134.6, 134.5, 132.3, 131.7, 131.4, 130.4, 130.2, 128.7, 125.7, 119.0, 32.0, 22.8. MS (ES): m/z 435.0 (M+). Anal. calcd. for C21H15ClN6OS.0.65C2H6O.0.1H2O: C, 57.40; H, 4.13; Cl, 7.60; N, 18.01; S, 6.87. Found: C, 57.11; H, 3.96; Cl, 7.45; N, 17.79; S, 6.90.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08138195B2 |
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| 출처 데이터셋 | uspto-grants-2012_03 |
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| ORD ID | ord-db707e8cb1044044930a7ffb1a7a852f |
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| 출처 메모 | uspto-grants-2012_03 |
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