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Hydrochloric Acid → HCID 67854283, 화합물

HRID 1655326
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HRID 1655326 반응식
[CH3:1][CH:2]([CH3:24])[CH2:3][CH2:4][CH:5]([NH:14][CH2:15][CH2:16][CH2:17][N:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1)[CH:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[OH:7].[H-].[Na+].S(C1C=CC(C)=CC=1)(O[CH3:31])(=O)=O.[ClH:39]>C1(C)C=CC=CC=1.CC(C)=O>[ClH:39].[ClH:39].[CH3:31][O:7][CH:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH:5]([NH:14][CH2:15][CH2:16][CH2:17][N:18]1[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]1)[CH2:4][CH2:3][CH:2]([CH3:24])[CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6645Methyl p-toluenesulfonateHCID 24758Sodium hydrideHCID 128308alpha-(4-Methyl-1-((3-(1-piperidinyl)propyl)amino)pentyl)benzenemethanol

생성물 1

HCID 67854283HCID 67854283, 화합물수율 21%

시약·촉매·용매 2

HCID 180
Acetone
용매
HCID 1140Toluene용매

실험 절차

To a solution of (1RS,2SR)-5-methyl-1-phenyl-2-(3-piperidinopropylamino)hexan-1-ol (1.66 g, 5 mmol) in toluene (25 ml) was added sodium hydride (0.14 g, 6 mmol) and the mixture was refluxed for 1 hour. To the reaction mixture was added methyl tosylate (1.12 g, 6 mmol) and the resulting mixture was refluxed for further 1 hour. After being cooled, the mixture was washed twice with water and once with brine, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by neutral alumina column chromatography (alumina: 40 g, eluent: chloroform) to give 1.1 g of oily matter. To a solution of the matter in acetone (20 ml) was added concentrated hydrochloric acid (0.1 ml) and the mixture was concentrated under reduced pressure. The residue was recrystallized from acetone (10 ml)-ethanol (0.2 ml) to obtain 0.45 g of the title compound as white crystals (yield: 21%).

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperaturethe resulting mixture was refluxed for further 1 hour
  3. temperatureAfter being cooled
  4. washthe mixture was washed twice with water and once with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by neutral alumina column chromatography (alumina: 40 g, eluent: chloroform)
  8. customto give 1.1 g of oily matter
  9. concentrationthe mixture was concentrated under reduced pressure
  10. customThe residue was recrystallized from acetone (10 ml)-ethanol (0.2 ml)

출처 및 근거

ORD 기록
ord-aabc9d85e47e46cba8039f597fdfbfe0
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05250546

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