참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Imidazole | HCID 795 | — |
| 반응물 | 5-Amino-2-fluoropyridine | HCID 819440 | — |
| 반응물 | 5-Amino-6-nitro-1H-isoindole-1,3(2H)-dione | HCID 15144568 | — |
| 용매 | Diphenyl Ether | HCID 7583 | — |
| 생성물 | 5-Amino-2-(6-fluoropyridin-3-yl)-6-nitroisoindoline-1,3-dione | HCID 66687151 | 12.7% |
반응 단계
5-Amino-6-nitroisoindoline-1,3-dione (2.00 g, 9.66 mmol), 6-fluoropyridin-3-amine (3.25 g, 28.98 mmol) and imidazole (1.32 g, 19.32 mmol) were suspended in diphenyl ether (50 mL). The mixture was stirred and heated to 200° C. for 24 h under argon. Then, the solid was filtered, washed with hexanes and purified by column chromatography (silica-gel, CH2Cl2/Acetone=7/3 v/v) to give a yellow solid product, 0.37 g, 12.7% yield. MS: 300.8 [M−H]−. 1H NMR (DMSO-d6, 500 MHz): δ 8.47 (s, 2H), 8.45 (s, 1H), 8.13-8.06 (m, 1H), 8.34 (d, 1H, J=2.1 Hz), 7.56 (s, 1H), 7.41 (dd, 1H, J1=8.7 Hz, J2=3.0 Hz).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08822500B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-d011ab5cde6d449083a8c9e244904952 |
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| 출처 메모 | uspto-grants-2014_09 |
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