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HRID 232827作成日:2026年10月25日
Trifluoroacetic acid → 3-((2-((7-Chloro-6-fluoro-2-quinolinyl)methoxy)-6,11-dihydrodibenz(b,E)oxepin-11-yl)thio)propanoic acid, (+)-
https://huagongshe.com/reaction/232827
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 3-Mercaptopropionic Acid | HCID 6514 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-11-hydroxy-6,11-dihydrodibenz[b,e]oxepine | HCID 23359134 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-((2-((7-Chloro-6-fluoro-2-quinolinyl)methoxy)-6,11-dihydrodibenz(b,E)oxepin-11-yl)thio)propanoic acid, (+)- | HCID 9849210 | 52.4% |
反応手順
While stirring under ice cooling, 1 g of 2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-11-hydroxy-6,11-dihydrodibenz[b,e]oxepine was added to a mixed solution of 8 ml of trifluoroacetic acid and 6 ml of methylene chloride, then 0.25 g of 3-mercaptopropionic acid was added to the solution and the mixture was stirred under ice cooling for 2 hours. After completion of the reaction, 180 ml of ice water was added the mixture, the mixture was adjusted to about pH 3 with a 1N-sodium hydroxide aqueous solution and then the aqueous layer was extracted with 200 ml of methylene chloride. The organic layer was washed with water and dried over anhydrous sodium sulfate and the residue obtained by removing the solvent under reduced pressure was recrystallized from ethyl acetate to obtain 0.63 g of the title compound as white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05591752 |
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| 出典データセット | uspto-grants-1997_01 |
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| ORD ID | ord-809e2ba3351b4b1e86813c9d52a6b680 |
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| 出典メモ | uspto-grants-1997_01 |
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