Hydrochloric Acid → (2S,3S)-2-phenylpiperidin-3-amine

HRID 2293708ノート

反応式

HRID 2293708 の反応式
[NH2:1][C:2]1[C:3]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[N:4][CH:5]=[CH:6][CH:7]=1.Cl.[H][H].O>CO.[Pt]>[NH2:1][C@H:2]1[CH2:7][CH2:6][CH2:5][NH:4][C@H:3]1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 27627843-Amino-2-phenylpyridineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 9812908(2S,3S)-2-phenylpiperidin-3-amine収率 87.3%

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 887Methanol溶媒

実験手順

In a bottle were placed 2.65 g (15.6 mmol) of 3-amino-2-phenylpyridine, 10.6 g of 5% platinum/carbon and 106 mL of 1.5 M HCl in methanol. The mixture was shaken under an atmosphere (ca. 40 p.s.i.) of hydrogen for 2.5 hours. Water was added to the system, the mixture was filtered through a pad of diatomaceous earth and the pad was rinsed with ca. 700 mL of water. The filtrate was made basic with solid sodium hydroxide and extracted with two portions of dichloromethane. The combined organic fractions were washed with water, dried (sodium sulfate) and concentrated with a rotary evaporator to obtain 2.4 g of the title compound as a yellow oil.

後処理

  1. filtrationthe mixture was filtered through a pad of diatomaceous earth
  2. washthe pad was rinsed with ca. 700 mL of water
  3. extractionextracted with two portions of dichloromethane
  4. washThe combined organic fractions were washed with water
  5. dry with materialdried (sodium sulfate)
  6. concentrationconcentrated with a rotary evaporator

出典と根拠

ORDレコード
ord-586596cf710c4a03b1a0ecba0ce21f4f
出典データセット
uspto-grants-1997_11
特許番号
US05686615

反応ノート

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