참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Formamidine acetate | HCID 160693 | — |
| 반응물 | 4-Fluoro-5-iodo-isatoic Anhydride | HCID 54335776 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178419030 | HCID 178419030 | 91.2% |
반응 단계
Dimethylformamide (0.5 litres), 4-fluoro-5-iodo-isatoic anhydride (45 grams, 147 mmoles), and formamidine acetate (45.92 grams, 441 mmoles), were combined in a one litre one-neck flask fitted with a magnetic stir bar. The mixture was placed under anhydrous nitrogen and heated at 110° C. for 6 hours. The mixture was allowed to cool, followed by concentrating the reaction mixture to one third its original volume on the rotary evaporator. The resulting mixture was poured onto 3 litres of ice water. The resulting precipitated solid was collected by suction filtration. The solid was washed with an additional one litre of distilled water. The resulting solid was dried under vacuum at 70° C. to yield 38.9 grams (91%) of the title compound. 1H NMR (400 MHz, DMSO-d6) δ: 12.43(s, 1H), 8.46(d, 1H), 8.12(s, 1H), 7.49(d, 1H). ESI-MS m/z 291 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07084147B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-0d4cdbe90b8748d0ab8949e429a5dc83 |
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| 출처 메모 | uspto-grants-2006_08 |
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