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HRID 1603285생성일: 2026년 10월 26일

Chloroform → 2-Methylthio-2,2,2',4'-tetrafluoroacetophenone

https://huagongshe.com/reaction/1603285

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참여 물질

역할이름HCID투입량
반응물ChloroformHCID 6212—
반응물HexaneHCID 8058—
반응물N-Fluoro-4-methylpyridinium-2-sulfonateHCID 2737404—
반응물1-(2,4-Difluorophenyl)-2-fluoro-2-(methylsulfanyl)ethanoneHCID 10632701—
용매1,1,2-TrichloroethaneHCID 6574—
생성물2-Methylthio-2,2,2',4'-tetrafluoroacetophenoneHCID 1022034747.5%

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온도100 °C

반응 단계

In a 20 ml solution of 0.5 g (2.3 mmol) of 2-methylthio-2,2',4'-trifluoroacetophenone [Compound (2b-1)] in 1,1,2-trichloroethane, 0.7 g (3.7 mmol) of N-fluoro-4-methylpyridinium-2-sulfonate ("MEC-02", trade name; Daikin Industries, Ltd.) was added at an internal temperature of 80° C., followed by stirring at an internal temperature of 100° C. for 20 minutes. After cooling, the reaction mixture was added to n-hexane. The insoluble matter so precipitated was filtered off. The insoluble matter was then washed with ethyl ether, followed by combination with the hexane layer. The layers so combined were washed successively with water and saturated saline, followed by drying over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure. The residue so obtained was subjected to chromatography on a silica gel column using chloroform, whereby 0.26 g of the title Compound (2c-1) was obtained in the form of a light yellow oil (yield: 48.1%).

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US05986144
출처 데이터셋uspto-grants-1999_11
ORD IDord-9ff763c582c047de971aa0222fe2b9e3
출처 메모uspto-grants-1999_11