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

HRID 512463노트

반응식

HRID 512463 반응식
[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

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 69233637HCID 69233637, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4f076c617179471f92cab9f88e7137f8
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09102623B2

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