Hydrochloric Acid → HCID 57749103、化合物
反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([CH3:8])[C:5]([C:9]([O:11]CC)=[O:10])=[N:4]1)[CH3:2].[OH-].[Na+].C(O)C.Cl>O>[CH2:1]([N:3]1[CH:7]=[C:6]([CH3:8])[C:5]([C:9]([OH:11])=[O:10])=[N:4]1)[CH3:2]参加物
6
実験手順
A mixture of ethyl 1-ethyl-4-methyl-1H-pyrazole-3-carboxylate (8.60 g, 47.2 mmol), 8N aqueous sodium hydroxide solution (11.8 mL) and ethanol (30 mL) was stirred at room temperature for 15 hr. The reaction mixture was neutralized with 1N hydrochloric acid, diluted with water, and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, and the residue was collected by filtration and washed with ethyl acetate-hexane to give the title compound (5.19 g, 71%) as a white solid.
後処理
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltrated
- concentrationThe filtrate was concentrated under reduced pressure
- filtrationthe residue was collected by filtration
- washwashed with ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-17a7ef7db9dc465f94bef9147f15a75f
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08304557B2
反応ノート
読み込み中…