4-(Aminomethyl)piperidine → 4-[2,4-Dimethyl-1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentylaminomethyl]piperidine

HRID 258785

반응식

HRID 258785 반응식
[CH3:1][CH:2]([C:13](=O)[CH:14]([CH3:25])[CH2:15]C1C(C)(C)C2CC1CC2)[CH2:3][CH:4]1[C:9]([CH3:11])([CH3:10])[CH:8]2[CH2:12][CH:5]1[CH2:6][CH2:7]2.[NH2:27][CH2:28][CH:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1.[H][H]>O=[Pt]=O.C(O)C>[CH3:25][CH:14]([CH:13]([NH:27][CH:28]([CH:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1)[CH:4]1[C:9]([CH3:11])([CH3:10])[CH:8]2[CH2:12][CH:5]1[CH2:6][CH2:7]2)[CH:2]([CH3:1])[CH2:3][CH:4]1[C:9]([CH3:11])([CH3:10])[CH:8]2[CH2:12][CH:5]1[CH2:6][CH2:7]2)[CH3:15]

참가 물질

6

반응물 3

HCID 235274-(Aminomethyl)piperidineHCID 214257072,4-Dimethyl-1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentanoneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 681236934-[2,4-Dimethyl-1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentylaminomethyl]piperidine

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 702Ethanol용매

실험 절차

A mixture of 2,4-dimethyl-1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentanone (g., 0.1 mole) and 4-aminomethylpiperidine (34.2 g., 0.3 mole) ml. ethanol is hydrogenated with PtO2 at room temperature and 40 psi hydrogen pressure. The 2.5 g. platinum catalyst is filtered off and the ethanol removed under reduced pressure. The residual oil is dissolved in ether and the ether solution washed several times with water to remove the excess 4-aminomethylpiperidine. The ether extracts are dried over anhydrous sodium sulfate and concentrated under vacuum to leave 4-[2,4-dimethyl-1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentylaminomethyl]piperidine.

후처리

  1. filtrationplatinum catalyst is filtered off
  2. customthe ethanol removed under reduced pressure
  3. dissolutionThe residual oil is dissolved in ether
  4. washthe ether solution washed several times with water
  5. customto remove the excess 4-aminomethylpiperidine
  6. dry with materialThe ether extracts are dried over anhydrous sodium sulfate
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-ecd5d6c851ed49639d779e2f14a35b3b
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04033748

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