Hydrochloric Acid → 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxylic acid
反応式
[F:1][CH:2]([F:13])[C:3]1[C:7]([C:8](F)=[O:9])=[C:6]([F:11])[N:5]([CH3:12])[N:4]=1.[OH-:14].[Na+].Cl>S1(=O)(=O)CCCC1>[F:11][C:6]1[N:5]([CH3:12])[N:4]=[C:3]([CH:2]([F:13])[F:1])[C:7]=1[C:8]([OH:14])=[O:9]参加物
5
実験手順
67.5 g of a solution (10% molar) of 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carbonyl fluoride in tetrahydrothiophene-1,1-dioxide were added dropwise to 400 mL of an aqueous 1N NaOH solution. During the addition, the temperature was kept below 20. After 2 h of stirring at room temperature, the mixture was carefully acidified to pH 2 using concentrated hydrochloric acid. The white precipitate formed was filtered off, washed with water and dried. This gave 6 g of 5-fluoro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid as a white solid.
後処理
- additionDuring the addition
- customThe white precipitate formed
- filtrationwas filtered off
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-2e8eac26822d4cdba49f3706a4b6e762
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09206137B2
反応ノート
読み込み中…