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Hydrochloric Acid → 2-(Fluoromethyl)piperazine dihydrochloride

HRID 1648658
ノート
印刷プレビュー

反応式

HRID 1648658 の反応式
C([N:8]1[CH2:13][CH2:12][N:11](CC2C=CC=CC=2)[CH2:10][CH:9]1[CH2:21][F:22])C1C=CC=CC=1.[H][H].[ClH:25]>CO.[Pd]>[ClH:25].[ClH:25].[F:22][CH2:21][CH:9]1[CH2:10][NH:11][CH2:12][CH2:13][NH:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 144794991,4-Dibenzyl-2-(fluoromethyl)piperazineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 144795022-(Fluoromethyl)piperazine dihydrochloride

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of a solution of 23.85 g (0.08 mole) of 1,4-dibenzyl-2-fluoromethylpiperazine [prepared as described in step (c) above] in 500 ml of methanol and 33 ml of concentrated aqueous hydrochloric acid was stirred vigorously at room temperature for 1 hour in an atmosphere of hydrogen and in the presence of 1.0 g of 20% w/w palladium-on-carbon. At the end of this time, the catalyst was removed by filtration and washed with water. The filtrate and washings were concentrated by evaporation under reduced pressure, and the residue was dissolved in 200 ml of water. The resulting aqueous solution was washed vigorously with ethyl acetate and separated. The aqueous layer was concentrated by evaporation under reduced pressure, and the residue was washed with ethanol to afford 13.76 g of 2-fluoromethylpiperazine dihydrochloride as a colorless powder, melting at 205°-218° C.

後処理

  1. customAt the end of this time, the catalyst was removed by filtration
  2. washwashed with water
  3. concentrationThe filtrate and washings were concentrated by evaporation under reduced pressure
  4. dissolutionthe residue was dissolved in 200 ml of water
  5. washThe resulting aqueous solution was washed vigorously with ethyl acetate
  6. customseparated
  7. concentrationThe aqueous layer was concentrated by evaporation under reduced pressure
  8. washthe residue was washed with ethanol

出典と根拠

ORDレコード
ord-c221cfdebc9c4161b9bc59561ff48598
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05436367

反応ノート

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