Hydrochloric Acid → 2-Phenylpiperidin-3-amine

HRID 2304530노트

반응식

HRID 2304530 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]>[Pt].O>[NH2:1][CH:2]1[CH2:7][CH2:6][CH2:5][NH:4][CH:3]1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

6

반응물 3

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

생성물 1

HCID 97940082-Phenylpiperidin-3-amine

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 962Water용매

실험 절차

A 500 ml Parr bottle was charged with 5 grams of 5% platinum/carbon (50% water wet), 5 grams (0.0293 mol.) 3-amino-2-phenylpyridine (1 equivalent), 75 ml of water (15 vol.) and 25 ml of concentrated hydrochloric acid (5 vol.). The reaction was hydrogenated (maintaining the hydrogen pressure between 36 psi and 50 psi) until high pressure liquid chromatography (HPLC) indicated complete reaction. The catalyst was removed by filtration and the pH of the filtrate was adjusted from 0 to a stable 11.2 using 25% sodium hydroxide (NaOH). The aqueous layer was extracted twice with 50 ml of methylene chloride (CH2Cl2). The organic extracts were combined, dried with magnesium sulfate (MgSO4) and the filtrate was atmospherically distilled to an oil, 4.34 grams (84.1%).

후처리

  1. customreaction
  2. customThe catalyst was removed by filtration
  3. extractionThe aqueous layer was extracted twice with 50 ml of methylene chloride (CH2Cl2)
  4. dry with materialdried with magnesium sulfate (MgSO4)
  5. distillationthe filtrate was atmospherically distilled to an oil, 4.34 grams (84.1%)

출처 및 근거

ORD 기록
ord-e83416b75ac34e70b7facdde71557728
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06436961B1

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