Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.Cl.[NH2:9][OH:10].S([O-])([O-])(=O)=O.[Na+].[Na+].[N+:18]([C:21]1[CH:27]=[CH:26][CH:25]=[CH:24][C:22]=1[NH2:23])([O-:20])=[O:19]>O.Cl>[OH:10][N:9]=[CH:2][C:3]([NH:23][C:22]1[CH:24]=[CH:25][CH:26]=[CH:27][C:21]=1[N+:18]([O-:20])=[O:19])=[O:5]
A solution of chloral hydrate (29 g, 175 mmol), hydroxylamine hydrochloride (69.4 g, 1000 mmol) and anhydrous sodium sulphate (21 g, 149 mmol) in water (800 mL) was heated to 65° C. To this a suspension, 2-nitroaniline (20 g, 150 mmol) in 2 molar aqueous HCl (20 mL) was added. This mixture was stirred overnight at the same temperature, then cooled to room temperature. The precipitated product was collected by filtration, washed with water dried in a vacuum oven to give 25 g of the required product as a yellow coloured solid (83%).
読み込み中…
