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

HRID 10597
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 10597
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
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

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

Produkt 1

HCID 21979764N-[(5-isoquinolyl)sulfonyl]-1,3-cyclohexanediamineAusbeute 108,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-3eab5bbdfa2e416eae1d6d8b01877451
Quelldatensatz
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07094789B2

Notizen zur Reaktion

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