1,3-Diamino-2-propanol → 1-Amino-3-[1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentylamino]-2-propanol

HRID 462327

반응식

HRID 462327 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][CH:27]([OH:30])[CH2:28][NH2:29].[H][H]>C(O)C.[Pt]=O>[NH2:25][CH2:26][CH:27]([OH:30])[CH2:28][NH:29][CH:11]([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)[CH2:10][CH2:9][CH:3]1[C:2]([CH3:24])([CH3:1])[CH:7]2[CH2:8][CH:4]1[CH2:5][CH2:6]2

참가 물질

6

반응물 3

HCID 611571,3-Diamino-2-propanolHCID 213328461,5-Di-(3,3-dimethylnorborn-2-yl)-3-pentanoneHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 213906211-Amino-3-[1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentylamino]-2-propanol

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 702Ethanol용매2회

실험 절차

A solution of 1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentanone (13.2 g., 0.04 mole) in 50 cc of anhydrous ethanol is added dropwise over about 20 minutes to a stirred solution of 1,3-diamino-2-hydroxypropane (25 g., 0.27 mole) in 200 cc of ethanol. The resulting mixture is then heated at reflux for about two hours, allowed to cool, 1.0 g. platinum oxide added, and the mixture reduced under a 40 psi hydrogen atmosphere until hydrogen uptake ceases. The mixture is then filtered from the catalyst, concentrated in vacuo to remove the ethanol, the oily residue taken up in ether (250 cc.), washed with water, dried over sodium sulfate, filtered and concentrated in vacuo to yield the product 1-amino-3-[1,5-di-(3,3-dimethylnorborn-2-yl)-3-pentylamino]-2-propanol as a pale yellow oil.

후처리

  1. temperatureThe resulting mixture is then heated
  2. temperatureat reflux for about two hours
  3. temperatureto cool
  4. filtrationThe mixture is then filtered from the catalyst
  5. concentrationconcentrated in vacuo
  6. customto remove the ethanol
  7. washwashed with water
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-578e89c8bb154f0f84c922b4c7af9d3e
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04065497

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