反応式
C(=O)(OC)[O:2][C:3]1[CH:8]=[CH:7][C:6]([F:9])=[C:5]([NH:10][C:11]([C:13]2[N:17]([CH3:18])[N:16]=[C:15]([CH3:19])[CH:14]=2)=[O:12])[CH:4]=1.[OH-].[Na+].Cl>CO>[F:9][C:6]1[CH:7]=[CH:8][C:3]([OH:2])=[CH:4][C:5]=1[NH:10][C:11]([C:13]1[N:17]([CH3:18])[N:16]=[C:15]([CH3:19])[CH:14]=1)=[O:12]参加物
5
実験手順
To a solution of 3-{[(1,3-dimethyl-1H-pyrazol-5-yl)carbonyl]amino}-4-fluorophenyl methyl carbonate (448 mg, 1.46 mmol) in methanol (10 mL) was added 1N aqueous sodium hydroxide solution (2 mL, 2 mmol) under ice-cooling, and the mixture was stirred at room temperature for 40 min. Under ice-cooling, 1N hydrochloric acid was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and filtrated. The solvent was evaporated under reduced pressure, and the residue was recrystallized from diethyl ether/hexane to give the title compound (305 mg, 84%) as a white powder.
後処理
- temperaturecooling
- temperatureUnder ice-cooling
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltrated
- customThe solvent was evaporated under reduced pressure
- customthe residue was recrystallized from diethyl ether/hexane
出典と根拠
- ORDレコード
- ord-a442603633d94c50b59a8e34eb647eb1
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08044049B2
関連ノート
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