Sodium Hydroxide → HCID 86600909, 화합물

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[NH2:1][C:2]1[C:3]([C:19]([NH2:21])=[O:20])=[N:4][C:5]([C:9]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([CH:16]([CH3:18])[CH3:17])[N:10]=2)=[CH:6][N+:7]=1[O-].[OH-].[Na+].P(Cl)(Cl)([Cl:26])=O>CN(C=O)C>[NH2:1][C:2]1[C:3]([C:19]([NH2:21])=[O:20])=[N:4][C:5]([C:9]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([CH:16]([CH3:18])[CH3:17])[N:10]=2)=[C:6]([Cl:26])[N:7]=1

참가 물질

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온도: 2.5 °C

실험 절차

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).