Potassium Carbonate → HCID 117770718, 화합물

HRID 1526387

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HRID 1526387 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][NH:6][C:5](=[O:9])[C:4]=1[C:10]#[N:11].[F:12][C:13]1[CH:14]=[C:15]([CH:18]=[C:19]([F:22])[C:20]=1F)[C:16]#[N:17].C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])O.[Na+]>CN(C)C=O>[C:16]([C:15]1[CH:14]=[C:13]([F:12])[C:20]([N:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]2=[O:9])=[C:19]([F:22])[CH:18]=1)#[N:17]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 5938143,4,5-TrifluorobenzonitrileHCID 27867023-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo-

생성물 1

HCID 117770718HCID 117770718, 화합물수율 43.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

A mixture of 4-methoxy-2-oxo-1,2-dihydropyridine-3-carbonitrile (2.00 g), 3,4,5-trifluorobenzonitrile (2.93 g), potassium carbonate (3.68 g) and N,N-dimethylformamide (20 mL) was stirred at 50° C. for 5 hr. The reaction mixture was slowly poured into saturated sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. To the residue was added a mixed solvent (10 mL) of isopropyl ether/ethyl acetate=4/1, and the mixture was stirred for 15 min. The precipitate was collected by filtration to give the title compound (1.65 g).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. additionTo the residue was added a mixed solvent (10 mL) of isopropyl ether/ethyl acetate=4/1
  6. stirringthe mixture was stirred for 15 min
  7. filtrationThe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-4a47bf8505ac4472bc43a66e5f332700
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085578B2

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