Diethyl Ether → 5-Difluoromethympyrazine-2-carboxylic acid

HRID 217983노트

반응식

HRID 217983 반응식
FC(F)(F)C(O)=O.[F:8][CH:9]([F:23])[C:10]1[N:11]=[CH:12][C:13]([C:16]([O:18]C(C)(C)C)=[O:17])=[N:14][CH:15]=1.CCOCC.[OH-].[Na+]>ClCCl>[F:23][CH:9]([F:8])[C:10]1[N:11]=[CH:12][C:13]([C:16]([OH:18])=[O:17])=[N:14][CH:15]=1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 57475685t-Butyl 5-difluoromethylpyrazine-2-carboxylate

생성물 1

HCID 574685755-Difluoromethympyrazine-2-carboxylic acid수율 75.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (1 mL) was added to a solution of t-butyl 5-difluoromethylpyrazine-2-carboxylate (175 mg) in dichloromethane (1 mL), and the mixture was stirred at room temperature for five hours. Ether and 5 N sodium hydroxide were added to the reaction solution. The aqueous layer was separated and made acidic with 5 N hydrochloric acid. Ethyl acetate was added to the aqueous layer, and the organic layer was separated. The organic layer was dried over anhydrous magnesium sulfate, and the insoluble matter was separated by filtration. The filtrate was concentrated to obtain the title compound (100 mg).

후처리

  1. customThe aqueous layer was separated
  2. additionEthyl acetate was added to the aqueous layer
  3. customthe organic layer was separated
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customthe insoluble matter was separated by filtration
  6. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-f129575f933b4192b3efdb3812efb555
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198269B2

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