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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

反応式

関与物質

役割名称HCID仕込み量
反応物Trifluoroacetic acidHCID 6422—
反応物3-Mercaptopropionic AcidHCID 6514—
反応物Sodium HydroxideHCID 14798—
反応物2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-11-hydroxy-6,11-dihydrodibenz[b,e]oxepineHCID 23359134—
溶媒DichloromethaneHCID 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 984921052.4%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US05591752
出典データセットuspto-grants-1997_01
ORD IDord-809e2ba3351b4b1e86813c9d52a6b680
出典メモuspto-grants-1997_01