참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Bromoacetamide | HCID 69632 | — |
| 반응물 | HCID 178448739 | HCID 178448739 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178448741 | HCID 178448741 | 49.2% |
반응 단계
To a solution of 2-Butyl-5-hydroxy-4-(7-hydroxy-1,1-dioxo-1,2-dihydro-1λ6-benzo[1,2,4]thiadiazin-3-yl)-6-isopropyl-2H-pyridazin-3-one (5f) (38.7 mg, 95.2 μmol) in anhydrous DMF (4 mL), 2-Bromo-acetamide (14.5 mg, 104.7 μmol) was added followed by K2CO3 (39.5 mg, 285.6 μmol). The resulted mixture was heated at 80° C. overnight with stirring. The reaction mixture was concentrated under reduced vacuum and the residue was purified by flash chromatography on silica gel to give the desired product (5g) (21.7 mg) in 49.2% yield. 1H NMR (400 MHz, DMSO-d6): δ7.63-7.66 (m, 1H), 7.62 (br, 1 H), 7.40 (br, 1H), 7.34-7.39 (m, 2 H), 4.58 (s, 2H), 4.10 (m, 2H), 3.23 (m, 1H, J=6.8 Hz), 1.72 (m, 2H, J=7.2 Hz), 1.32 (m, 2H. J=7.2 Hz), 1.21 (d, 6H, J=6.4 Hz), 0.91 (t, 3H, J=7.2 Hz); LC-MS (ESI+): m/e=464.1-[M+1]+ (exact MS: 463.15).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07425552B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-d8afea77e3c245abb45d6f1465c7d0da |
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| 출처 메모 | uspto-grants-2008_09 |
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