HCID 66783884、化合物 → HCID 86611476、化合物

HRID 1844828ノート

反応式

HRID 1844828 の反応式
[Br-].[F:2][C:3]([F:8])([F:7])[C:4]([Zn+])=[CH2:5].[Br:9][C:10]1[C:11]([O:17][CH:18]([F:20])[F:19])=[C:12](I)[CH:13]=[CH:14][CH:15]=1>O1CCCC1.Cl>[Br:9][C:10]1[C:11]([O:17][CH:18]([F:20])[F:19])=[C:12]([C:4]([C:3]([F:8])([F:7])[F:2])=[CH2:5])[CH:13]=[CH:14][CH:15]=1

参加物

5

反応物 2

HCID 66783884HCID 66783884、化合物HCID 178477747HCID 178477747、化合物

生成物 1

HCID 86611476HCID 86611476、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In 10 ml of a solution of 1-trifluoromethylethenyl zinc bromide prepared according to the method described in documents in 1M tetrahydrofuran, 1.0 g of 3-bromodifluoromethoxy-1-iodobenzene and 0.05 g of dichlorobis(triphenylphosphine) palladium (II) were added, and stirred under reflux with heat for 2 hours. After the completion of the reaction, the reaction mixture was poured in 20 ml of diluted hydrochloric acid, extracted with ethyl acetate (50 ml×1). The organic phase was dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. The residue was dissolved in hexane, and high polar impurities were excluded by treating with silica gel to obtain 0.77 g of crude aimed product as colorless oily substance. The resulting product was used as such without purification for the next step.

後処理

  1. temperatureunder reflux
  2. temperaturewith heat for 2 hours
  3. customAfter the completion of the reaction
  4. extractionextracted with ethyl acetate (50 ml×1)
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. dissolutionThe residue was dissolved in hexane
  8. additionby treating with silica gel

出典と根拠

ORDレコード
ord-f675171d89ef47b3b9051b432f885331
出典データセット
uspto-grants-2015_02
特許番号
US08946492B2

反応ノート

読み込み中…