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Hydrochloric Acid → 6-(Dimethylamino)-5-methyl-3-pyridinecarboxylic acid

HRID 502424
ノート
印刷プレビュー

反応式

HRID 502424 の反応式
[CH3:1][N:2]([CH3:12])[C:3]1[C:10]([CH3:11])=[CH:9]C(C#N)=[CH:5][N:4]=1.[OH-].[Na+].Cl.C1C[O:19]CC1.[CH2:21]([OH:23])[CH3:22]>>[CH3:1][N:2]([CH3:12])[C:3]1[C:10]([CH3:11])=[CH:9][C:22]([C:21]([OH:19])=[O:23])=[CH:5][N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21873804Tetrahydrofuran ethanolHCID 68455945HCID 68455945、化合物

生成物 1

HCID 684549596-(Dimethylamino)-5-methyl-3-pyridinecarboxylic acid

実験手順

The above prepared 6-dimethylamino-5-methyl-nicotinonitrile (0.435 g, 2.70 mmol) was dissolved in 13.6 ml of THF/ethanol=1/1 and treated with 6.75 ml of 2N NaOH (5 eq.). The mixture was refluxed for 30 h; aliquots were taken from time to time and analyzed by MS to follow the disappearance of the amide intermediate. After cooling down to room temperature, the pH was adjusted with HCl to 3. Careful evaporation of the solvents and drying under HV left 1.45 g of the title acid as white solid, contaminated with NaCl, which was used as such for the next step.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureThe mixture was refluxed for 30 h
  2. customCareful evaporation of the solvents
  3. customdrying under HV
  4. waitleft 1.45 g of the title acid as white solid

出典と根拠

ORDレコード
ord-129956e00932491ca0f2fc902c01cffa
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07772253B2

反応ノート

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