Potassium Carbonate → HCID 86750964, 화합물

HRID 1683807노트

반응식

HRID 1683807 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:12][C:11](=[O:13])[NH:10][N:9]=2)=[CH:4][CH:3]=1.Cl[CH2:15][C:16](=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH2:12][C:11](=[O:13])[N:10]([CH2:15][C:16](=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18])[N:9]=2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 835721-ChloropinacoloneHCID 47787935-(4-Chloro-phenyl)-2,4-dihydro-pyrazol-3-one

생성물 1

HCID 86750964HCID 86750964, 화합물수율 104.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 3.5 g (16 mmol) of 3-(4-chlorophenyl)-4, 5-dihydropyrazol-5-one, 2.9 g (24 mmol) of chloropinacolone, 5.4 g (39 mmol) of anhydrous potassium carbonate and acetonitrile was heated under reflux for 14 hours. Excess potassium carbonate and the formed salts were removed by filtration. The filtrate was concentrated and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1 (v/v)) to give 4.9 g of the object compound as white crystals (yield 97%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 14 hours
  3. customExcess potassium carbonate and the formed salts were removed by filtration
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1 (v/v))

출처 및 근거

ORD 기록
ord-ebf881da69db4ec6a2346067fc959a9b
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05639776

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