関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 3-(7-Benzyloxy-6-methoxy-quinolin-4-yloxy)-5,6-dimethyl-[2,3']bipyridine | HCID 57756571 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 4-(5,6-Dimethyl-[2,3']bipyridin-3-yloxy)-6-methoxy-quinolin-7-ol | HCID 136131618 | 120% |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560558B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-95373be0265540349abc74a32492fac4 |
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| 出典メモ | uspto-grants-2009_07 |
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