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

HRID 1439312

反応式

HRID 1439312 の反応式
[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

参加物

6

反応物 3

HCID 611571,3-Diamino-2-propanolHCID 213328461,5-Di-(3,3-dimethylnorborn-2-yl)-3-pentanoneHCID 178418361HCID 178418361、化合物2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 702Ethanol溶媒2 回

実験手順

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 2 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.

後処理

  1. temperatureThe resulting mixture is then heated
  2. temperatureat reflux for about 2 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

出典と根拠

ORDレコード
ord-0941ac10129d4675bfbf7ecb6b15fd7d
出典データセット
uspto-grants-1977_11
特許番号
US04058625

関連ノート

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