Water → HCID 86598208, 화합물

HRID 2217255노트

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HRID 2217255 반응식
[NH2:1][C:2]1[N:3]=[C:4]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:5]([C:14]2[CH:15]=[CH:16][C:17](=[O:23])[N:18]([CH:20]([CH3:22])[CH3:21])[CH:19]=2)=[N:6][C:7]=1[C:8]#[C:9][Si](C)(C)C.C([O-])([O-])=O.[K+].[K+].O.CCOC(C)=O>CO>[NH2:1][C:2]1[N:3]=[C:4]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:5]([C:14]2[CH:15]=[CH:16][C:17](=[O:23])[N:18]([CH:20]([CH3:22])[CH3:21])[CH:19]=2)=[N:6][C:7]=1[C:8]#[CH:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 69103390HCID 69103390, 화합물

생성물 1

HCID 86598208HCID 86598208, 화합물수율 40.6%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
25 °C

실험 절차

A mixture of 5-{5-amino-3-phenyl-6-[(trimethylsilyl)ethynyl]-2-pyrazinyl}-1-isopropyl-2(1H)-pyridone (300 mg) and sat. K2CO3 in MeOH (4.5 ml) was stirred at 25° C. for 3 hours. Water and EtOAc were poured into the mixture, and the organic layer was separated, washed with water and brine, and dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by short column (silica-gel; CH2Cl2) and recrystallized from EtOH to give 5-(5-amino-6-ethynyl-3-phenyl-2-pyrazinyl)-1-isopropyl-2(1H)-pyridone (100 mg).

후처리

  1. customthe organic layer was separated
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed under reduced pressure
  5. customThe residue was purified by short column (silica-gel; CH2Cl2)
  6. customrecrystallized from EtOH

출처 및 근거

ORD 기록
ord-e7304bafd9dc40f08cabe2ff1347945f
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07407961B2

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