HCID 23002992, Verbindung → HCID 66618157, Verbindung

HRID 2093556Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2093556
[BrH:1].C(O)C.[NH2:5][C:6]1[C:7]2[C:8]3[C:9](=[N:21][N:22]([CH2:24][C:25]4[C:30]([Cl:31])=[C:29]([O:32][CH3:33])[C:28]([CH3:34])=[CH:27][N:26]=4)[N:23]=2)[CH:10]=[C:11]([CH2:16][C:17]([NH:19][CH3:20])=[O:18])[C:12]=3[CH2:13][S:14][N:15]=1>C(#N)C>[BrH:1].[NH2:5][C:6]1[C:7]2[C:8]3[C:9](=[N:21][N:22]([CH2:24][C:25]4[C:30]([Cl:31])=[C:29]([O:32][CH3:33])[C:28]([CH3:34])=[CH:27][N:26]=4)[N:23]=2)[CH:10]=[C:11]([CH2:16][C:17]([NH:19][CH3:20])=[O:18])[C:12]=3[CH2:13][S:14][N:15]=1

Komponenten

4

Edukt 2

HCID 23002992HCID 23002992, VerbindungHCID 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 66618157HCID 66618157, VerbindungAusbeute 48,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A 20% hydrobromic acid-ethanol solution (204 μl, 0.505 mmol) was added to an acetonitrile solution (350 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 (250 mg, 0.561 mmol) at room temperature. The resulting mixture was stirred for 3 hours, and the precipitated solid was then collected by filtration. Ethanol (3 ml) was added to the resulting solid, and the resulting mixture was then stirred for 1 day. Thereafter, the solid was collected by filtration. The solid was then dried under reduced pressure at room temperature for 2 days, so as to obtain the title compound (128 mg, 0.243 mmol).

Aufarbeitung

  1. filtrationthe precipitated solid was then collected by filtration
  2. additionEthanol (3 ml) was added to the resulting solid
  3. stirringthe resulting mixture was then stirred for 1 day
  4. filtrationThereafter, the solid was collected by filtration
  5. customThe solid was then dried under reduced pressure at room temperature for 2 days

Quellen und Nachweise

ORD-Eintrag
ord-de7fd8c92dc3472cb3586667fb2f7e6e
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08445504B2

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