Ethanol → HCID 18768043, Verbindung

Reaktionsgleichung

S(S([O-])=O)([O-])=O.[Na+].[Na+].[NH:9]([C:16]1[C:21]([Br:22])=[CH:20][N:19]=[C:18]([NH:23][C:24]2[CH:29]=[CH:28][C:27]([N+:30]([O-])=O)=[CH:26][CH:25]=2)[N:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(O)C>O>[NH2:30][C:27]1[CH:28]=[CH:29][C:24]([NH:23][C:18]2[N:17]=[C:16]([NH:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:21]([Br:22])=[CH:20][N:19]=2)=[CH:25][CH:26]=1

Komponenten

Versuchsvorschrift

Sodium hydrosulphite (9.5 g, 54.5 mmol) was added over 30 minutes to a stirred solution of anilino-5-bromo-2-(4-nitroanilino)pyrimidine (Method 39; 7.0 g, 18.2 mmol) in a hot mixture of ethanol and water (1:1, 100 ml). The resulting suspension was stirred for a further two hours and insoluble material was removed by filtration. The filtrate was concentrated and the residue was partitioned between 1M aqueous sodium hydroxide (50 ml), and DCM (100 ml). The organic layer was separated, washed with water (2×10 ml) and dried. Volatile material was removed by evaporation to give the product (4.55 g, 70%). MS (MH+): 356, 358.