Hydrochloride methanol → Methyl 3-cyclopropylpyridine-2-carboxylate
反応式
[CH:1]1([C:4]2[C:5]([C:10]([OH:12])=[O:11])=[N:6][CH:7]=[CH:8][CH:9]=2)[CH2:3][CH2:2]1.Cl.[CH3:14]O>>[CH:1]1([C:4]2[C:5]([C:10]([O:12][CH3:14])=[O:11])=[N:6][CH:7]=[CH:8][CH:9]=2)[CH2:2][CH2:3]1参加物
3
実験手順
830 mg of a hydrochloride salt of the 3-cyclopropylpyridine-2-carboxylic acid [121-3] was dissolved in 100 mL of 10% hydrochloric acid-methanol solution, and heated overnight under reflux. The reaction solution was concentrated under reduced pressure, a saturated aqueous solution of sodium hydrogen carbonate was added to the obtained residue, and was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The insolubles were filtered, the filtrate was concentrated under reduced pressure, and 363 mg of methyl 3-cyclopropylpyridine-2-carboxylate [121-4] was obtained as a white solid.
後処理
- temperatureheated overnight
- temperatureunder reflux
- concentrationThe reaction solution was concentrated under reduced pressure
- additiona saturated aqueous solution of sodium hydrogen carbonate was added to the obtained residue
- extractionwas extracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- filtrationThe insolubles were filtered
- concentrationthe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-35cad4f5ba5e4f2885be1ebfb664c756
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07718801B2
反応ノート
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