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

HRID 1436119
ノート
印刷プレビュー

反応式

HRID 1436119 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-64f80dfbc92942a0b11281ed60e8a623
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07618960B2

反応ノート

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