Sodium Hydroxide → 5-bromo-1-tert-butyl-1H-pyrazole-4-carboxylic acid
反応式
[Br:1][C:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:5]=[CH:4][C:3]=1[C:11]([O:13]CC)=[O:12].[OH-].[Na+]>C(O)C.C1COCC1>[Br:1][C:2]1[N:6]([C:7]([CH3:8])([CH3:9])[CH3:10])[N:5]=[CH:4][C:3]=1[C:11]([OH:13])=[O:12]参加物
5
実験手順
A mixed solution of the compound (13.5 g, 49.07 mmol) obtained in step 2 and 1N aqueous sodium hydroxide solution (65 mL, 65.00 mmol) in ethanol (70 mL) and THF (70 mL) was stirred at 60° C. for 2.5 hr. The organic solvent was evaporated under reduced pressure, and water and 1N hydrochloric acid (70 mL) were added thereto. The precipitate was collected by filtration, and washed with diethyl ether and hexane to give 5-bromo-1-tert-butyl-1H-pyrazole-4-carboxylic acid (10.29 g, 41.6 mmol, 85%) as a white powder.
後処理
- customThe organic solvent was evaporated under reduced pressure, and water and 1N hydrochloric acid (70 mL)
- additionwere added
- filtrationThe precipitate was collected by filtration
- washwashed with diethyl ether and hexane
出典と根拠
- ORDレコード
- ord-4b4d8d18a2cf4c4f98ea3d4c1637599e
- 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…