Butyl bromide → HCID 59234227, 화합물

HRID 1400203노트

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HRID 1400203 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].Br[CH2:13][CH2:14][CH2:15][CH3:16].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:13]([N:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]1=[O:9])[CH2:14][CH2:15][CH3:16]

참가 물질

5

반응물 3

HCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 27867023-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo-

생성물 1

HCID 59234227HCID 59234227, 화합물수율 99.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
110 °C

실험 절차

To a solution of 4-methoxy-2-oxo-1,2-dihydro-pyridine-3-carbonitrile (20 g, 133 mmol) in acetonitrile (800 ml) were added 1-bromobutane (15.8 ml, 146 mmol) and potassium carbonate (36.7 g, 266 mmol) and the mixture was heated at 110° C. for 24 hours. The mixture was cooled to room temperature and the solid was filtered off The filtrate was evaporated till dryness and the resulting crude residue was then triturated with diethylether to yield pure intermediate 4 (27.39 g, >99%) as a white solid.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationthe solid was filtered off The filtrate
  3. customwas evaporated till dryness
  4. customthe resulting crude residue was then triturated with diethylether

출처 및 근거

ORD 기록
ord-2d3089667ecd46d0abd5110fe40970dd
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08906939B2

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