참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Phenol, 4-amino-2-fluoro- | HCID 2735918 | — |
| 반응물 | 4-Chloro-1H-pyrrolo[2,3-b]pyridine | HCID 11389493 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-((1H-Pyrrolo[2,3-B]pyridin-4-YL)oxy)-3-fluoroaniline | HCID 16037965 | — |
반응 단계
543 mg (3.56 mmol) of 4-chloro-1H-pyrrolo[2,3-b]pyridine (from example XVIII, 905 mg (7.12 mmol) of 3-fluoro-4-hydroxyaniline and 399 mg (7.12 mmol) of powdered potassium hydroxide are heated at 260° C. for 8 hours. Another 905 mg (7.12 mmol) of 3-fluoro-4-hydroxyaniline and 200 mg (3.56 mmol) of powdered potassium hydroxide are added, and the mixture is reacted at 260° C. for another 8 h. For work-up, the mixture is cooled to room temperature, diluted with water and extracted three times with ethyl acetate. The organic phase is dried over magnesium sulfate and concentrated using a rotary evaporator. The residue is purified by preparative HPLC. The fractions which, according to LC-MS, contain 39% of product are used without further purification for the next reaction.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07737153B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-e1ae06632b2441b793d7925135e5427b |
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| 출처 메모 | uspto-grants-2010_06 |
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