Sodium Hydroxide → 1-Isobutyl-2-oxo-1,2-dihydropyridine-4-carboxylic acid

HRID 2192484ノート

反応式

HRID 2192484 の反応式
[OH-].[Na+].[CH3:3][CH:4]([CH3:17])[CH2:5][N:6]1[CH:11]=[CH:10][C:9]([C:12]([O:14]C)=[O:13])=[CH:8][C:7]1=[O:16]>CO>[CH3:3][CH:4]([CH3:17])[CH2:5][N:6]1[CH:11]=[CH:10][C:9]([C:12]([OH:14])=[O:13])=[CH:8][C:7]1=[O:16]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 59214340HCID 59214340、化合物

生成物 1

HCID 446005741-Isobutyl-2-oxo-1,2-dihydropyridine-4-carboxylic acid収率 95.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 2M aqueous solution of sodium hydroxide (5.38 ml, 10.75 mmol) was added to a solution of methyl 1-(2-methylpropyl)-2-oxo-1,2-dihydro-4-pyridinecarboxylate (D27; 0.45 g, 2.151 mmol) in methanol (10 ml). The mixture was stirred at room temperature for 2 hrs and then the solvent was removed under vacuum. The residue was taken up with water, neutralised with 2M HCl and extracted with ethyl acetate. The organic layer was washed with water, dried over magnesium sulphate and concentrated under vacuum to give the title compound as a white solid (400 mg).

後処理

  1. customthe solvent was removed under vacuum
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-80a094f04e5c448c801008136ebf029e
出典データセット
uspto-grants-2012_12
特許番号
US08329730B2

反応ノート

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