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1,4-Dioxane hydrochloride → 6-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one hydrochloride monohydrate

HRID 1847031
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1847031
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([N:7]=[CH:8][C:9](=[O:34])[N:10]2[CH2:13][CH2:14][CH2:15][NH:16][C@H:17]2[CH2:21][N:20]([C:22]3[CH:23]=[CH:24][C:25]4[O:30][CH2:29][C:28](=[O:31])[NH:27][C:26]=4[CH:32]=3)[C:19](=[O:33])[CH2:18]2)=[CH:5][CH:4]=1.[ClH:35].O1CCOCC1>ClCCl.C(O)C>[OH2:2].[ClH:35].[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([N:7]=[CH:8][C:9](=[O:34])[N:10]2[CH2:13][CH2:14][CH2:15][NH:16][C@H:17]2[CH2:21][N:20]([C:22]3[CH:23]=[CH:24][C:25]4[O:30][CH2:29][C:28](=[O:31])[NH:27][C:26]=4[CH:32]=3)[C:19](=[O:33])[CH2:18]2)=[CH:5][CH:4]=1
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Komponenten

5

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 601617766-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one

Produkt 1

HCID 867249586-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one hydrochloride monohydrateAusbeute 147,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

6-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one (2.86 g, 6.17 mmol) was dissolved in dichloromethane (50 ml) and ethanol (2 ml). To this solution was added 4 N hydrogen chloride/dioxane solution (1.59 ml, 6.37 mmol) under cooling in an ice bath. The precipitated insoluble material was collected by filtration and was then dried. The obtained residue was suspended in ethanol (20 ml), and the suspension was then stirred at 50° C. for 20 minutes. The suspension was cooled in an ice bath, and the insoluble material was collected by filtration. The filtrate was dried at 70° C. overnight under reduced pressure to yield 2.36 g (74%) of the above-captioned compound in the form of a colorless solid.

Aufarbeitung

  1. temperatureunder cooling in an ice bath
  2. filtrationThe precipitated insoluble material was collected by filtration
  3. customwas then dried
  4. temperatureThe suspension was cooled in an ice bath
  5. filtrationthe insoluble material was collected by filtration
  6. customThe filtrate was dried at 70° C. overnight under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-bc610aeabd144bb3b3db35a1e5778625
Quelldatensatz
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08952010B2

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