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HRID 1646987作成日:2026年10月26日

Hydrochloric Acid → 8-fluoro-3-(4-fluorophenyl)-2,3-dihydro-4H-1-benzothiopyran-4-one

https://huagongshe.com/reaction/1646987

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物Aluminum(III) ChlorideHCID 6451240—
反応物4-Fluoro-alpha-[[(2-fluorophenyl)thio]methyl]benzeneacetic acidHCID 19927556—
溶媒Thionyl ChlorideHCID 24386—
生成物8-fluoro-3-(4-fluorophenyl)-2,3-dihydro-4H-1-benzothiopyran-4-oneHCID 1973675082%

反応条件

温度0 °C

反応手順

The acid from Step C (4.5 g, 15 mmole) was dissolved in 30 ml of thionyl chloride and refluxed for four hours. After cooling the thionyl chloride was concentrated and the residue taken up in carbon tetrachloride. The carbon tetrachloride was concentrated and the residue was taken up in 30 ml of dichloroethane. To the dichloroethane solution being cooled in an ice bath, was added aluminum trichloride (total of 2.1 g, 16 mmole) in three portions every 15 min. After stirring the black solution for an additional 30 min at 0° C., a 5% aqueous HCl solution was added. The aqueous phase was separated and extracted twice with methylene chloride. The organic phases were combined, dried (MgSO4), and concentrated to give the crude product as a yellow oil (3.4 g, 82% yield).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05182303
出典データセットuspto-grants-1993_01
ORD IDord-0a4260efac9d41d8ad0b12ffbc8a1e52
出典メモuspto-grants-1993_01