Potassium Carbonate → 4',4-Dichlorochalcone

HRID 2379305

反応式

HRID 2379305 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14]S(F)(=O)=O)=[CH:10][CH:9]=1.[Cl:19][C:20]1[CH:29]=[CH:28][C:23]([C:24](=[O:27])[CH2:25]Br)=[CH:22][CH:21]=1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1>[Cl:19][C:20]1[CH:29]=[CH:28][C:23]([C:24](=[O:27])/[CH:25]=[CH:14]/[C:11]2[CH:12]=[CH:13][C:8]([Cl:7])=[CH:9][CH:10]=2)=[CH:22][CH:21]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 68303p-Chlorophenacyl bromideHCID 18958404HCID 18958404、化合物

生成物 1

HCID 53770114',4-Dichlorochalcone収率 68.7%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A catalytic amount (about 300 mg) of tetrabutylammonium bromide and 68 g of powdered anydrous potassium carbonate were added to a solution of 21.8 g 4-chlorophenylmethanesulphonyl fluoride and 23.3 g of 4-chlorophenacyl bromide in 200 ml of tetrahydrofuran at room temperature, while stirring. The mixture was stirred for a further 8 hours at 50° C. The reaction mixture was allowed to cool down to room temperature and was then filtered to remove inorganic substances which had precipitated. The organic phase was concentrated by stripping off the solvent under reduced pressure. The residue was recrystallized from ethanol. In this manner, 19.0 g of trans-1,3-di-(4-chlorophenyl)-prop-2-en-1-one were obtained in the form of yellow crystals of melting point 156° C.

後処理

  1. stirringThe mixture was stirred for a further 8 hours at 50° C
  2. filtrationwas then filtered
  3. customto remove inorganic substances which
  4. customhad precipitated
  5. concentrationThe organic phase was concentrated
  6. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-8d838e072ffe4b74bc4706278c196e33
出典データセット
uspto-grants-1994_11
特許番号
US05360935

関連ノート

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