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

HRID 258785

反応式

HRID 258785 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ecd5d6c851ed49639d779e2f14a35b3b
出典データセット
uspto-grants-1977_07
特許番号
US04033748

関連ノート

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