참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phenylacetic Acid | HCID 999 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 반응물 | 2-amino-4-morpholinophthalazin-1(2H)-one | HCID 70976104 | — |
| 생성물 | N-[4-(morpholin-4-yl)-1-oxophthalazin-2(1H)-yl]-2-phenylacetamide | HCID 70976253 | — |
반응 단계
To a 4 mL vial was added the product from Example 1B (20 mg in dimethyl acetamide), phenylacetic acid [1.5 equivalents in dimethyl acetamide], O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HATU, 2 equivalents in dimethyl acetamide) and triethylamine (3 equivalents, neat). The vial was capped and microwaved at 150° C. for 30 minutes. The reaction was checked by LC/MS and concentrated to dryness upon completion. The residue was dissolved in 1:1 MeOH:DMSO and purified by reverse phase HPLC (conditions from Example 10C): 1H NMR (500 MHz, DMSO-d6/D2O) δ 8.33-8.28 (m, 1H), 8.03 (d, J=7.5, 1H), 8.01-7.96 (m, 1H), 7.94-7.87 (m, 1H), 7.40-7.33 (m, 4H), 7.33-7.25 (m, 1H), 3.86-3.78 (m, 4H), 3.67 (s, 2H), 3.11-3.06 (m, 4H); MS (ESI+) M/Z 365 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08859549B2 |
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| 출처 데이터셋 | uspto-grants-2014_10 |
|---|
| ORD ID | ord-18bf992b4f04433fac641294f2b4bc7e |
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| 출처 메모 | uspto-grants-2014_10 |
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