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

反応式

[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

参加物

反応物 2

HCID 24386Thionyl Chloride

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

生成物 1

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

実験手順

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.

後処理

temperatureAfter cooling down
customthe reaction mixture is evaporated under vacuum

出典と根拠

ORDレコード: ord-2ae406a1b1f44ba186aa057025e54866
出典データセット: uspto-grants-2016_01
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09232799B2

反応ノート

読み込み中…

参加物