Potassium Carbonate → HCID 86750964、化合物

HRID 1683807ノート

反応式

HRID 1683807 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 86750964HCID 86750964、化合物収率 104.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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))

出典と根拠

ORDレコード
ord-ebf881da69db4ec6a2346067fc959a9b
出典データセット
uspto-grants-1997_06
特許番号
US05639776

反応ノート

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