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Water → (S)-1-(3,4,5-Trifluorophenyl)ethan-1-amine

HRID 1436119
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HRID 1436119 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[N:20]([C@H:23]([C:25]1[CH:26]=[C:27]([F:33])[C:28]([F:32])=[C:29]([F:31])[CH:30]=1)[CH3:24])=[N+]=[N-].O>C1COCC1>[F:31][C:29]1[CH:30]=[C:25]([C@@H:23]([NH2:20])[CH3:24])[CH:26]=[C:27]([F:33])[C:28]=1[F:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 866126155-((S)-1-azidoethyl)-1,2,3-trifluorobenzene

생성물 1

HCID 51358460(S)-1-(3,4,5-Trifluorophenyl)ethan-1-amine수율 46.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Triphenylphosphine (1.23 g) was added to a solution of 5-((S)-1-azidoethyl)-1,2,3-trifluorobenzene (858 mg) in THF (20 ml) in a nitrogen atmosphere, and the reaction solution was stirred at room temperature for five minutes. Thereafter, water (2.5 ml) was added to the reaction solution, which was then stirred at 60° C. for 2.5 hours. The reaction solution was returned to room temperature, followed by extraction with 2 N hydrochloric acid (twice). The hydrochloric acid extraction layer was washed with ethyl acetate and then made basic with a 5 N sodium hydroxide solution, followed by extraction with methylene chloride (twice). The methylene chloride layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to obtain 348 mg of the title compound. Further, the following operation was performed in order to collect the title compound remaining in the ethyl acetate dilution of the reaction solution. Diethyl ether was added to the dilution, followed by extraction with water. The water extraction layer was washed with diethyl ether and then made basic with a 5 N sodium hydroxide solution, followed by extraction with methylene chloride (twice). The methylene chloride layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to obtain 413 mg of the title compound.

후처리

  1. stirringwas then stirred at 60° C. for 2.5 hours
  2. customwas returned to room temperature
  3. extractionfollowed by extraction with 2 N hydrochloric acid (twice)
  4. extractionThe hydrochloric acid extraction layer
  5. washwas washed with ethyl acetate
  6. extractionfollowed by extraction with methylene chloride (twice)
  7. dry with materialThe methylene chloride layer was dried over anhydrous magnesium sulfate
  8. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-64f80dfbc92942a0b11281ed60e8a623
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618960B2

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