Sodium Hydroxide → HCID 86600909, Verbindung

To a suspension 3-amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinecarboxamide 4-oxide (1.65 g) in DMF (33 ml), phosphorous oxychloride (1.59 ml) was added below −30° C. and the mixture was stirred at 0-5° C. for one hour. The reaction mixture was poured into ice-water (132 ml), stirred at 40-50° C. for 2 hours, adjusted to pH 8 with 30% aq. NaOH solution under ice-cooling and a precipitate was collected by filtration. The precipitate was purified by column chromatography on silica gel eluting with a mixture of MeOH and EtOAc (2:98 v/v) to give 3-amino-5-chloro-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinecarboxamide as a solid (682 mg).

1. stirringstirred at 40-50° C. for 2 hours
2. temperaturecooling
3. filtrationa precipitate was collected by filtration
4. customThe precipitate was purified by column chromatography on silica gel eluting with a mixture of MeOH and EtOAc (2:98 v/v)

ORD-Eintrag

ord-fc43b84bdb5748c5bac854fd43d5fbca

Quelldatensatz

uspto-grants-2007_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07265120B2