Potassium Carbonate → HCID 117770282, 화합물

HRID 1526383

반응식

HRID 1526383 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:18]=[C:17]([N+:19]([O-:21])=[O:20])[CH:16]=[C:15]([F:22])[C:14]=1F.C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])O.[Na+]>CN(C)C=O>[F:12][C:13]1[CH:18]=[C:17]([N+:19]([O-:21])=[O:20])[CH:16]=[C:15]([F:22])[C:14]=1[N:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]1=[O:9]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 27827931,2,3-Trifluoro-5-nitrobenzeneHCID 27867023-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo-

생성물 1

HCID 117770282HCID 117770282, 화합물수율 91.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4-methoxy-2-oxo-1,2-dihydropyridine-3-carbonitrile (2.00 g), 1,2,3-trifluoro-5-nitrobenzene (3.54 g), potassium carbonate (3.73 g) and N,N-dimethylformamide (20 mL) was stirred at room temperature for 2 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 (3.75 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-66bece1a3d6f4fbd87ecc70b68d925b8
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085578B2

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