Potassium Carbonate → HCID 20286598、化合物

HRID 127239

反応式

HRID 127239 の反応式
Br[CH2:2][C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][Cl:6].[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:6][CH2:5][C:4]([CH3:8])([CH3:7])[C:3](=[O:9])[CH2:2][O:23][C:20]1[CH:19]=[CH:18][C:17]([C:14]2[CH:15]=[CH:16][C:11]([Cl:10])=[CH:12][CH:13]=2)=[CH:22][CH:21]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 915894'-Chloro-4-biphenylolHCID 104207672-Butanone, 1-bromo-4-chloro-3,3-dimethyl-

生成物 1

HCID 20286598HCID 20286598、化合物収率 55.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

42.7 g (0.2 mol) of 1-bromo-4-chloro-3,3-dimethyl-butan-2-one were added dropwise to a boiling suspension of 41 g (0.2 mol) of 4-(4-chlorophenyl)-phenol and 28 g (0.2 mol) of potassium carbonate in 300 ml of absolute acetone. The mixture was stirred for 15 hours under reflux and was then allowed to cool and the inorganic residue was filtered off and rinsed with acetone. The filtrate was concentrated by distilling off the solvent in vacuo. The residue crystallized after the addition of 50 ml of diisopropyl ether. 37.5 g (55% of theory) of 4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-butan-2-one of melting point 67°-68° C. were obtained.

後処理

  1. temperatureunder reflux
  2. temperatureto cool
  3. filtrationthe inorganic residue was filtered off
  4. washrinsed with acetone
  5. concentrationThe filtrate was concentrated
  6. distillationby distilling off the solvent in vacuo
  7. customThe residue crystallized
  8. additionafter the addition of 50 ml of diisopropyl ether

出典と根拠

ORDレコード
ord-68c453afb2d64ef2b7b89777c2689575
出典データセット
uspto-grants-1981_03
特許番号
US04255434

関連ノート

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