Potassium Iodide → HCID 117770038, 화합물

HRID 1526376

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HRID 1526376 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].C(=O)([O-])[O-].[Cs+].[Cs+].[I-].[K+].Br[CH:21]([CH2:23][CH3:24])[CH3:22]>C(=O)([O-])O.[Na+].COCCOC>[CH:21]([N:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]1=[O:9])([CH2:23][CH3:24])[CH3:22]

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 65542-BromobutaneHCID 10796Cesium carbonateHCID 27867023-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo-

생성물 1

HCID 117770038HCID 117770038, 화합물수율 48%

시약·촉매·용매 2

HCID 80711,2-Dimethoxyethane용매HCID 516892Sodium Bicarbonate용매

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온도
60 °C

실험 절차

To a mixture of 4-methoxy-2-oxo-1,2-dihydropyridine-3-carbonitrile (500 mg), cesium carbonate (2.17 g), potassium iodide (553 mg) N,N-dimethylformamide (10 mL) and 1,2-dimethoxyethane (10 mL) was added 2-bromobutane (776 mg) at room temperature, and the mixture was stirred overnight at 60° C. The reaction mixture was diluted with saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted threetimes with ethyl acetate. The extracts were combined, washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (330 mg).

후처리

  1. extractionthe mixture was extracted threetimes with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-9d34407f90f241f1a9266b80a887fca7
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085578B2

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