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Sodium Hydroxide → HCID 13671866, 화합물

HRID 1655325
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HRID 1655325 반응식
[NH2:1][CH:2]([CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4].[ClH:16].S(C1C=CC(C)=CC=1)(O[CH2:21][CH2:22][CH2:23][N:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1)(=O)=O.C(=O)(O)[O-].[Na+].[OH-].[Na+]>C(O)C.O.CCOCC>[ClH:16].[ClH:16].[CH3:14][CH:13]([CH3:15])[CH2:12][CH2:11][CH:2]([NH:1][CH2:21][CH2:22][CH2:23][N:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1)[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 13671865HCID 13671865, 화합물HCID 19791697HCID 19791697, 화합물

생성물 1

HCID 13671866HCID 13671866, 화합물수율 60%

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 962
Water
용매
HCID 3283Diethyl Ether용매

실험 절차

A mixture of (1RS,2SR)-2-amino-5-methyl-1-phenylhexan-1-ol (1.04 g, 5 mmol), 3-piperidinopropyl tosylate hydrochloride (2.00 g, 6 mmol) and sodium bicarbonate (1.05 g, 12.5 mmol) in ethanol (10 ml) was refluxed for 1 hour. After cooling, to the reaction mixture were added ether (100 ml), water (50 ml) and 2N-NaOH (5 ml) and the resulting mixture was well shaken. The ethereal layer was separated and washed three times with water, then once with brine, followed by drying and subsequent concentration under reduced pressure. The residue was dissolved in ethanol and to the solution was added 6N-HCl in EtOH (1.5 ml). Precipitated crystals were collected by filtration and then recrystallized from ethanol to obtain 0.73 g of the title compound as white crystals (yield: 36%).

후처리

  1. temperaturewas refluxed for 1 hour
  2. temperatureAfter cooling, to the reaction mixture
  3. customThe ethereal layer was separated
  4. washwashed three times with water
  5. customby drying
  6. concentrationsubsequent concentration under reduced pressure
  7. dissolutionThe residue was dissolved in ethanol and to the solution
  8. additionwas added 6N-HCl in EtOH (1.5 ml)
  9. customPrecipitated crystals
  10. filtrationwere collected by filtration
  11. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-985c44c167284781af9b5eb92d5754d8
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05250546

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