참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Lithium amide | HCID 24532 | — |
| 반응물 | 2-Fluoro-4-iodoaniline | HCID 185694 | — |
| 반응물 | 2,4,6-Trifluorobenzoic acid | HCID 520373 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 67051560 | HCID 67051560 | 59.2% |
반응 단계
2,4,6-Trifluorobenzoic acid (643 mg, 3.65 mmol) and 2-fluoro-4-iodoaniline (1.0 g, 4.22 mmol) were taken into acetonitrile (30 mL) followed by addition of lithium amide (290 mg, 12.7 mmol) and the mixture was heated to 60° C. under a nitrogen atmosphere for one hour. On cooling to room temperature the mixture was added to 1 N aqueous hydrochloric acid (100 mL) and the precipitate formed was collected by filtration and washed once with water then hexanes and dried in vacuo to give 2,4-difluoro-6-[(2-fluoro-4-iodophenyl)amino]benzoic acid (849 mg, 59% yield) as a tan solid. 1H-NMR (400 MHz, D6-DMSO): 13.72 (br s, 1H), 9.46 (s, 1H), 7.75 (d, 1H), 7.56 (d, 1H) 7.28 (tr, 1H), 6.73-6.67 (m, 1H), 6.53 (d, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07915250B2 |
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| 출처 데이터셋 | uspto-grants-2011_03 |
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| ORD ID | ord-0409980f7ea24b898c45b4a2ca38eb6b |
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| 출처 메모 | uspto-grants-2011_03 |
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