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1,4-Dioxane hydrochloride → N-{4-[2-(4-hydrazinocarbonylmethylphenyl)ethyl]phenyl}acetamide hydrochloride

HRID 1465434
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1465434
O1CCOCC1.[ClH:7].[C:8]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([CH2:26][C:27]([NH:29][NH:30]C(OC(C)(C)C)=O)=[O:28])=[CH:22][CH:21]=2)=[CH:14][CH:13]=1)(=[O:10])[CH3:9]>>[ClH:7].[NH:29]([C:27]([CH2:26][C:23]1[CH:22]=[CH:21][C:20]([CH2:19][CH2:18][C:15]2[CH:14]=[CH:13][C:12]([NH:11][C:8](=[O:10])[CH3:9])=[CH:17][CH:16]=2)=[CH:25][CH:24]=1)=[O:28])[NH2:30]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67030250Tert-butyl 2-({4-[(4-acetamidophenyl)ethyl]phenyl}acetyl)hydrazinecarboxylate

Produkt 1

HCID 67030104N-{4-[2-(4-hydrazinocarbonylmethylphenyl)ethyl]phenyl}acetamide hydrochlorideAusbeute 98 %

Versuchsvorschrift

4M-Hydrogen chloride dioxane solution (1 ml, 4 mmol) was added to tert-butyl 2-({4-[(4-acetamidophenyl)ethyl]phenyl}acetyl)hydrazinecarboxylate (23 mg, 0.056 mmol), and the mixture was stirred at room temperature for 15 mins. The reaction mixture was concentrated under reduced pressure, dichloromethane was added, and the mixture was concentrated again, and hydrogen chloride gas was removed. The precipitate was collected by filtration, washed with diethyl ether and dried under reduced pressure to give the title compound (18 mg, yield 98%) as a slightly yellow solid.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure, dichloromethane
  2. additionwas added
  3. concentrationthe mixture was concentrated again
  4. customhydrogen chloride gas was removed
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with diethyl ether
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cab499f9c9944612ae025fd8380c79e1
Quelldatensatz
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08999989B2

Notizen zur Reaktion

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