참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | 3-(7-Benzyloxy-6-methoxy-quinolin-4-yloxy)-5,6-dimethyl-[2,3']bipyridine | HCID 57756571 | — |
| 용매 | Trifluoroacetic acid | HCID 6422 | — |
| 생성물 | 4-(5,6-Dimethyl-[2,3']bipyridin-3-yloxy)-6-methoxy-quinolin-7-ol | HCID 136131618 | 120% |
반응 단계
3-(7-Benzyloxy-6-methoxy-quinolin-4-yloxy)-5,6-dimethyl-[2,3′]bipyridine (compound 344) (804 mg) was dissolved in trifluoroacetic acid (8 ml) to prepare a solution. Methanesulfonic acid (0.8 ml) was added to the solution, and the mixture was stirred at 70° C. for 1.5 hr. The reaction solution was cooled to room temperature, and the solvent was removed by distillation under the reduced pressure. An aqueous sodium hydrogencarbonate solution was then added to the residue, and the mixture was extracted with chloroform. The chloroform layer was washed with saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using chloroform-methanol to give the title compound (777 mg, yield 100%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07560558B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
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| ORD ID | ord-95373be0265540349abc74a32492fac4 |
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| 출처 메모 | uspto-grants-2009_07 |
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