Sodium Hydroxide → HCID 178524803、化合物
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:12]([C:13]([O:15]CC)=[O:14])=[CH:11][NH:10][N:9]=2)=[CH:4][CH:3]=1.[OH-].[Na+]>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:12]([C:13]([OH:15])=[O:14])=[CH:11][NH:10][N:9]=2)=[CH:6][CH:7]=1参加物
4
実験手順
To a solution of the compound (25.0 g, 107 mmol) obtained in step 2 in ethanol (90 mL) was added 2N aqueous sodium hydroxide solution (117 mL, 235 mmol) at room temperature, and the mixture was heated under reflux for 24 hr. The organic solvent was evaporated, and ethyl acetate was added to the residue. The aqueous layer was separated, and 2N hydrochloric acid was added until the aqueous layer became pH2. The precipitate was collected by filtration to give 3-(4-fluorophenyl)-1H-pyrazole-4-carboxylic acid (22.8 g, 100%) as a yellow powder.
後処理
- temperaturethe mixture was heated
- temperatureunder reflux for 24 hr
- customThe organic solvent was evaporated
- additionethyl acetate was added to the residue
- customThe aqueous layer was separated
- addition2N hydrochloric acid was added until the aqueous layer
- filtrationThe precipitate was collected by filtration
出典と根拠
- ORDレコード
- ord-b477207b7ab24fc08b9c69413b064667
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09156837B2
反応ノート
読み込み中…