Potassium Carbonate → HCID 59272909, 화합물

HRID 1400202

반응식

HRID 1400202 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].[CH:12]1([CH2:15][CH2:16]OS(C)(=O)=O)[CH2:14][CH2:13]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH:12]1([CH2:15][CH2:16][N:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]2=[O:9])[CH2:14][CH2:13]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27867023-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo-HCID 145578092-Cyclopropylethyl methanesulfonate

생성물 1

HCID 59272909HCID 59272909, 화합물수율 46%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
105 °C

실험 절차

To a solution of 4-methoxy-2-oxo-1,2-dihydro-pyridine-3-carbonitrile (19.81 g, 131.98 mmol) in acetonitrile (520 ml) were added intermediate 1 (34.36 g, 171.57 mmol) and potassium carbonate (56.73 g, 410.3 mmol) and the mixture was heated at 105° C. for 12 hours. The mixture was cooled to room temperature and the solid was filtered off The filtrate was evaporated till dryness. The crude product was purified by column chromatography (silica gel; DCM to DCM/EtOAc up to 20% as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 3 (13.18 g, 46%).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationthe solid was filtered off The filtrate
  3. customwas evaporated till dryness
  4. customThe crude product was purified by column chromatography (silica gel; DCM to DCM/EtOAc up to 20% as eluent)
  5. customThe desired fractions were collected
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-19baa36cf228409a8f37bc71082ba742
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08906939B2

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