Lithium Hydroxide → 6-(Difluoromethyl)-2-oxo-1,2-dihydropyridine-3-carboxylic acid

HRID 512463ノート

反応式

HRID 512463 の反応式
[F:1][CH:2]([F:14])[C:3]1[NH:8][C:7](=[O:9])[C:6]([C:10]([O:12]C)=[O:11])=[CH:5][CH:4]=1.[OH-].[Li+]>CO.O>[F:14][CH:2]([F:1])[C:3]1[NH:8][C:7](=[O:9])[C:6]([C:10]([OH:12])=[O:11])=[CH:5][CH:4]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 69233637HCID 69233637、化合物

生成物 1

HCID 685011126-(Difluoromethyl)-2-oxo-1,2-dihydropyridine-3-carboxylic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

7.4 g (36.4 mmol) of methyl 6-(difluoromethyl)-2-oxo-1,2-dihydropyridine-3-carboxylate were dissolved in 100 ml of methanol, and a solution of 1.3 g (54.6 mmol) of lithium hydroxide in 50 ml of water was added. After two hours of heating under reflux, the mixture was concentrated to a volume of about 50 ml and the solution was washed with dichloromethane. The aqueous phase was then acidified with 2N hydrochloric acid and extracted with ethyl acetate. Drying and concentration of the extract gave 5.6 g (82% of theory) of a brownish powder.

後処理

  1. temperatureAfter two hours of heating
  2. temperatureunder reflux
  3. concentrationthe mixture was concentrated to a volume of about 50 ml
  4. washthe solution was washed with dichloromethane
  5. extractionextracted with ethyl acetate
  6. customDrying
  7. customconcentration of the extract gave 5.6 g (82% of theory) of a brownish powder

出典と根拠

ORDレコード
ord-4f076c617179471f92cab9f88e7137f8
出典データセット
uspto-grants-2015_08
特許番号
US09102623B2

反応ノート

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