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1,4-Dioxane hydrochloride → N,N-bis(1H-imidazol-2-ylmethyl)-N'-(piperidin-4-ylmethyl)urea

HRID 1897632
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1897632
CN(C)S([N:6]1[CH:10]=[CH:9][N:8]=[C:7]1[CH2:11][N:12]([CH2:30][C:31]1[N:32](S(N(C)C)(=O)=O)[CH:33]=[CH:34][N:35]=1)[C:13]([NH:15][CH2:16][CH:17]1[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]1)=[O:14])(=O)=O.Cl.O1CCOCC1>>[NH:6]1[CH:10]=[CH:9][N:8]=[C:7]1[CH2:11][N:12]([CH2:30][C:31]1[NH:32][CH:33]=[CH:34][N:35]=1)[C:13]([NH:15][CH2:16][CH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)=[O:14]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67500244tert-butyl 4-[({[bis({1-[(dimethylamino)sulfonyl]-1H-imidazol-2-yl)methyl]amino}carbonyl)amino]methyl}piperidine-1-carboxylate

Produkt 1

HCID 67502645N,N-bis(1H-imidazol-2-ylmethyl)-N'-(piperidin-4-ylmethyl)urea

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To the compound (3.00 g) obtained in Example 9, 4N hydrogen chloride/dioxane (15 mL) was added. The reaction solution was stirred at 60° C. for 15 hours. The reaction solution was concentrated under reduced pressure. The residue was dissolved in methanol (20 mL) and a carbonate resin (trade name: MP-Carbonate, manufactured by Argonaut Co., product number: 800267, 10 g) was added, followed by stirring at room temperature for 3 hours. After the resin was removed by filtration, the filtrate was concentrated under reduced pressure. The title compound was obtained without purifying the residue.

Aufarbeitung

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in methanol (20 mL)
  3. additiona carbonate resin (trade name: MP-Carbonate, manufactured by Argonaut Co., product number: 800267, 10 g) was added
  4. stirringby stirring at room temperature for 3 hours
  5. customAfter the resin was removed by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9c00655d02874f19a712a819e4343779
Quelldatensatz
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08519124B2

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