Ethanol → 2-(Propan-2-yl)pyridine-4-carboxylic acid

HRID 1838250ノート

反応式

HRID 1838250 の反応式
[OH-:1].[K+].[CH2:3]([OH:5])[CH3:4].C(C1[CH:13]=[CH:12][N:11]=[C:10]([CH:14]([CH3:16])[CH3:15])[CH:9]=1)#N.O>C(OCC)C>[CH:14]([C:10]1[CH:9]=[C:4]([CH:13]=[CH:12][N:11]=1)[C:3]([OH:1])=[O:5])([CH3:16])[CH3:15]

参加物

6

反応物 4

HCID 702EthanolHCID 962WaterHCID 14797Potassium HydroxideHCID 1184982-(Isopropyl)isonicotinonitrile

生成物 1

HCID 225077152-(Propan-2-yl)pyridine-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A 7.5 ml portion of 8 N aqueous potassium hydroxide was added to 50 ml of ethanol solution containing 2.7 g of 4-cyano-2-isopropylpyridine, and the mixture was heated under reflux for 12 hours. After cooling to room temperature, the reaction mixture was mixed with water and diethyl ether and the aqueous layer was separated. The aqueous layer was adjusted to an acidic pH of 3 using 4 N hydrochloric acid and then saturated with sodium chloride. This was extracted with a mixed solvent of ethyl acetate-isopropanol (5:1, v/v) and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure to obtain 3.1 g of the title compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 12 hours
  3. customthe aqueous layer was separated
  4. extractionThis was extracted with a mixed solvent of ethyl acetate-isopropanol (5:1
  5. dry with materialv/v) and dried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ba4adcc6219246b7ac21553354cbd458
出典データセット
uspto-grants-2004_01
特許番号
US06673799B1

反応ノート

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