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Hydrochloric Acid → 1,4-Diazepan-5-one--hydrogen chloride (1/1)

HRID 1437244
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1437244
[ClH:1].C([N:9]1[CH2:15][CH2:14][C:13](=[O:16])[NH:12][CH2:11][CH2:10]1)C1C=CC=CC=1.[H][H]>C(O)C.CO.[C].[Pd]>[ClH:1].[NH:9]1[CH2:15][CH2:14][C:13](=[O:16])[NH:12][CH2:11][CH2:10]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 3

HCID 313Hydrochloric AcidHCID 2397261-Benzyl-1,4-diazepan-5-oneHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 230903691,4-Diazepan-5-one--hydrogen chloride (1/1)Ausbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418390HCID 178418390, VerbindungKatalysator
HCID 702
Ethanol
Lösungsmittel
HCID 887MethanolLösungsmittel

Versuchsvorschrift

1M HCl in ethanol (7.2 mL) and 10% palladium-carbon (0.34 g) were added to 1-benzylhexahydro-1H-1,4-diazepin-5-one (1.490 g) in methanol (10 mL) at room temperature, and the resultant mixture was stirred in a hydrogen atmosphere for 4 hours. After the reaction atmosphere was purged with nitrogen, insoluble matter was removed by filtration. The solvent of the filtrate was evaporated under reduced pressure, and diethyl ether was added to the residue, and then the precipitated solid was recovered by filtration, to thereby give the title compound (1.045 g, 96%).

Aufarbeitung

  1. customAfter the reaction atmosphere
  2. customwas purged with nitrogen, insoluble matter
  3. customwas removed by filtration
  4. customThe solvent of the filtrate was evaporated under reduced pressure, and diethyl ether
  5. additionwas added to the residue
  6. filtrationthe precipitated solid was recovered by filtration

Quellen und Nachweise

ORD-Eintrag
ord-fa7de088fada47f69ce40bd3dfec0682
Quelldatensatz
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07622471B2

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