Hydrochloric Acid → 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 hydrochloride

HRID 2408901Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2408901
Cl.[NH2:2][C:3]1[C:4]2[C:5]3[C:6](=[N:18][N:19]([CH2:21][C:22]4[C:27]([Cl:28])=[C:26]([O:29][CH3:30])[C:25]([CH3:31])=[CH:24][N:23]=4)[N:20]=2)[CH:7]=[C:8]([CH2:13][C:14]([NH:16][CH3:17])=[O:15])[C:9]=3[CH2:10][S:11][N:12]=1>C(O)C>[ClH:28].[NH2:2][C:3]1[C:4]2[C:5]3[C:6](=[N:18][N:19]([CH2:21][C:22]4[C:27]([Cl:28])=[C:26]([O:29][CH3:30])[C:25]([CH3:31])=[CH:24][N:23]=4)[N:20]=2)[CH:7]=[C:8]([CH2:13][C:14]([NH:16][CH3:17])=[O:15])[C:9]=3[CH2:10][S:11][N:12]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric 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 666180732-{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 hydrochlorideAusbeute 194,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

3 M hydrochloric acid (9.2 ml, 27.8 mmol) was added dropwise to an ethanol (200 ml) suspension 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 (5446.6 mg, 11.6 mmol) at 25° C., while the suspension was stirred. The resulting mixture was stirred for 3.5 hours. The obtained crystal was collected by filtration, was then washed with ethanol (50 ml), and was then dried under reduced pressure at 40° C. for 14 hours, so as to obtain the above title compound (5436.1 mg, 116. mmol). Yield: 99%.

Aufarbeitung

  1. stirringThe resulting mixture was stirred for 3.5 hours
  2. filtrationThe obtained crystal was collected by filtration
  3. washwas then washed with ethanol (50 ml)
  4. customwas then dried under reduced pressure at 40° C. for 14 hours

Quellen und Nachweise

ORD-Eintrag
ord-670d00eeee6f4f4b8a37dda5572fbe26
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08815880B2

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