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Hydrochloric Acid → N-[(5-isoquinolyl)sulfonyl]-1,3-cyclohexanediamine

HRID 10597
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인쇄 미리보기

반응식

HRID 10597 반응식
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH:11]([NH:15][S:16]([C:19]2[CH:28]=[CH:27][CH:26]=[C:25]3[C:20]=2[CH:21]=[CH:22][N:23]=[CH:24]3)(=[O:18])=[O:17])[CH2:10]1)=O)(C)(C)C.Cl>CO>[CH:24]1[C:25]2[C:20](=[C:19]([S:16]([NH:15][CH:11]3[CH2:12][CH2:13][CH2:14][CH:9]([NH2:8])[CH2:10]3)(=[O:17])=[O:18])[CH:28]=[CH:27][CH:26]=2)[CH:21]=[CH:22][N:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21979834N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-1,3-cyclohexanediamine

생성물 1

HCID 21979764N-[(5-isoquinolyl)sulfonyl]-1,3-cyclohexanediamine수율 108.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Intermediate 54 (6 g) obtained above was added to a 10% hydrogen chloride solution in methanol (50 ml) and stirred under reflux by heating for 1.5 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in a mixed solvent of dichloromethane and ethanol, added with saturated aqueous potassium carbonate and vigorously shaken. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain the title compound (4.9 g).

후처리

  1. temperatureunder reflux
  2. temperatureby heating for 1.5 hours
  3. customThe solvent was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in a mixed solvent of dichloromethane and ethanol
  5. additionadded with saturated aqueous potassium carbonate
  6. stirringvigorously shaken
  7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  8. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-3eab5bbdfa2e416eae1d6d8b01877451
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07094789B2

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