HCID 66783884, 화합물 → HCID 86611476, 화합물

HRID 910383노트

반응식

HRID 910383 반응식
[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

참가 물질

5

반응물 2

HCID 66783884HCID 66783884, 화합물HCID 178477747HCID 178477747, 화합물

생성물 1

HCID 86611476HCID 86611476, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-db076cc18b97483c8903aed7638a9b62
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022089B2

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