Diethyl Ether → HCID 86652177, Verbindung

HRID 2093558Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2093558
C(OCC)C.[CH3:6][S:7]([OH:10])(=[O:9])=[O:8].[NH2:11][C:12]1[C:13]2[C:14]3[C:15](=[N:27][N:28]([CH2:30][C:31]4[C:36]([Cl:37])=[C:35]([O:38][CH3:39])[C:34]([CH3:40])=[CH:33][N:32]=4)[N:29]=2)[CH:16]=[C:17]([CH2:22][C:23]([NH:25][CH3:26])=[O:24])[C:18]=3[CH2:19][S:20][N:21]=1>C(#N)C>[CH3:6][S:7]([OH:10])(=[O:9])=[O:8].[NH2:11][C:12]1[C:13]2[C:14]3[C:15](=[N:27][N:28]([CH2:30][C:31]4[C:36]([Cl:37])=[C:35]([O:38][CH3:39])[C:34]([CH3:40])=[CH:33][N:32]=4)[N:29]=2)[CH:16]=[C:17]([CH2:22][C:23]([NH:25][CH3:26])=[O:24])[C:18]=3[CH2:19][S:20][N:21]=1

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 666180742-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide

Produkt 1

HCID 86652177HCID 86652177, VerbindungAusbeute 88,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

A diethyl ether solution (50 ml) of methanesulfonic acid (32 mg, 0.302 mmol) was added at 5° C. to an acetonitrile solution (150 ml) of 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (151 mg, 0.339 mmol). The resulting mixture was stirred at 5° C. for 25 minutes. Thereafter, the solvent was distilled away under reduced pressure, an appropriate amount of diethyl ether was then added to the residue, and a solid was then collected by filtration. Thereafter, ethanol (1 ml) was added to the resulting solid, and the resulting mixture was then stirred at room temperature for approximately 1 day. Thereafter, a solid was collected by filtration, and it was then dried under reduced pressure at room temperature for 1 day, so as to obtain the title compound (145 mg, 0.268 mmol).

Aufarbeitung

  1. distillationThereafter, the solvent was distilled away under reduced pressure
  2. additionan appropriate amount of diethyl ether was then added to the residue
  3. filtrationa solid was then collected by filtration
  4. additionThereafter, ethanol (1 ml) was added to the resulting solid
  5. stirringthe resulting mixture was then stirred at room temperature for approximately 1 day
  6. filtrationThereafter, a solid was collected by filtration, and it
  7. customwas then dried under reduced pressure at room temperature for 1 day

Quellen und Nachweise

ORD-Eintrag
ord-78ceabf0b5684ae6889c2be4d9218c89
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08445504B2

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