Hydrochloride methanol → Methyl 3-cyclopropylpyridine-2-carboxylate

HRID 2238670ノート

反応式

HRID 2238670 の反応式
[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

  1. temperatureheated overnight
  2. temperatureunder reflux
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. additiona saturated aqueous solution of sodium hydrogen carbonate was added to the obtained residue
  5. extractionwas extracted with ethyl acetate
  6. washThe organic layer was washed with saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationThe insolubles were filtered
  9. 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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