1,3-Propanediamine → 1-[1,5-Di-(3,3-dimethylnorborn-2-yl)-3-pentyl]-1,5-diazapentane

HRID 1390553

반응식

HRID 1390553 반응식
[CH3:1][C:2]1([CH3:24])[CH:7]2[CH2:8][CH:4]([CH2:5][CH2:6]2)[CH:3]1[CH2:9][CH2:10][C:11](=O)[CH2:12][CH2:13][CH:14]1[C:19]([CH3:21])([CH3:20])[CH:18]2[CH2:22][CH:15]1[CH2:16][CH2:17]2.[NH2:25][CH2:26][CH2:27][CH2:28][NH2:29].C1(C)C=CC=CC=1>O>[CH3:1][C:2]1([CH3:24])[CH:7]2[CH2:8][CH:4]([CH2:5][CH2:6]2)[CH:3]1[CH2:9][CH2:10][CH:11]([NH:25][CH2:26][CH2:27][CH2:28][NH2:29])[CH2:12][CH2:13][CH:14]1[C:19]([CH3:21])([CH3:20])[CH:18]2[CH2:22][CH:15]1[CH2:16][CH2:17]2

참가 물질

5

반응물 3

HCID 4281,3-PropanediamineHCID 1140TolueneHCID 213328461,5-Di-(3,3-dimethylnorborn-2-yl)-3-pentanone

생성물 1

HCID 213328411-[1,5-Di-(3,3-dimethylnorborn-2-yl)-3-pentyl]-1,5-diazapentane

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1,5-Di-(3,3-dimethylnorborn-2-yl)-3-pentanone (6.04 g., 0.02 mole) and 1,3-diaminopropane (0.10 mole) in 150 ml. toluene is heated at reflux overnight with a Dean-Stark water separator. The cooled solution is concentrated under reduced pressure. The residue is dissolved in ethanol and hydrogenated with PtO2 at room temperature and 40 psi hydrogen pressure. The platinum catalyst is filtered off and the ethanol removed under vacuum. The residue is dissolved in ether and the ether solution washed several times with water to remove the excess 1,3-diaminopropane. The ether extracts are dried over anhydrous sodium sulfate and concentrated under vacuum to leave the diamine product, 1-[1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentyl]-1,5-diazapentane.

후처리

  1. concentrationThe cooled solution is concentrated under reduced pressure
  2. dissolutionThe residue is dissolved in ethanol and hydrogenated with PtO2 at room temperature
  3. filtrationThe platinum catalyst is filtered off
  4. customthe ethanol removed under vacuum
  5. dissolutionThe residue is dissolved in ether
  6. washthe ether solution washed several times with water
  7. customto remove the excess 1,3-diaminopropane
  8. dry with materialThe ether extracts are dried over anhydrous sodium sulfate
  9. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-4444781ecc344d81b16335c4fb2d12f8
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04139559

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