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

HRID 2293708노트

반응식

HRID 2293708 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 27627843-Amino-2-phenylpyridineHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-586596cf710c4a03b1a0ecba0ce21f4f
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05686615

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