Thionyl Chloride → 5-fluoro-1-methyl-3-difluoromethyl-1H-pyrazole-4-carbonyl chloride

반응식

[F:1][CH:2]([F:13])[C:3]1[C:7]([C:8](O)=[O:9])=[C:6]([F:11])[N:5]([CH3:12])[N:4]=1.S(Cl)([Cl:16])=O>>[F:1][CH:2]([F:13])[C:3]1[C:7]([C:8]([Cl:16])=[O:9])=[C:6]([F:11])[N:5]([CH3:12])[N:4]=1

참가 물질

반응물 2

HCID 24386Thionyl Chloride

HCID 231925843-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxylic acid

생성물 1

HCID 529205085-fluoro-1-methyl-3-difluoromethyl-1H-pyrazole-4-carbonyl chloride

실험 절차

9.1 g of 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxylic acid and 75.5 mL of thionyl chloride are refluxed for 1.5 hours. After cooling down, the reaction mixture is evaporated under vacuum to yield 10 g of 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carbonyl chloride as a yellow oil. GC-MS; observed M/z: Molecular ion: (M+.)=212; fragments: (M+.−Cl)=177 and (M+.−F)=193.

후처리

temperatureAfter cooling down
customthe reaction mixture is evaporated under vacuum

출처 및 근거

ORD 기록: ord-7de0443b8fce4302972c473d73880833
출처 데이터셋: uspto-grants-2016_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09320276B2

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