Hydrochloric Acid → HCID 21201126, Verbindung

Reaktionsgleichung

[N+:1]([C:4]1[CH:5]=[C:6]([CH:25]=[C:26]([N+:28]([O-])=O)[CH:27]=1)[C:7]([O:9][CH2:10][CH2:11][N:12]1[C:16](=[O:17])[CH:15]=[C:14]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:13]1=[O:24])=[O:8])([O-])=O.Cl.[OH-].[Na+]>O1CCOCC1>[NH2:28][C:26]1[CH:25]=[C:6]([CH:5]=[C:4]([NH2:1])[CH:27]=1)[C:7]([O:9][CH2:10][CH2:11][N:12]1[C:16](=[O:17])[CH:15]=[C:14]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:13]1=[O:24])=[O:8]

Komponenten

Versuchsvorschrift

In a 300 ml three-necked flask equipped with a dropping funnel and a stirring means were placed 8.22 g of N-(2-(3,5-dinitrobenzoyl)oxyethyl)-α-phenylmaleimide and 150 ml of dioxane, and 30.2 g of stannous chloride (dihydrate) was added at room temperature under stirring. Then, 30.2 g of conc. hydrochloric acid was added dropwise thereto, and thereafter, stirring was continued at room temperature for 3 hours. After completion of the reaction, a 2N aqueous solution of sodium hydroxide was added dropwise thereto until it was neutral, and the reaction solution was filtered with Celite. The filtrate was extracted twice with ethyl acetate, and the organic phase was washed three times with water and dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the filtrate was concentrated under reduced pressure to afford a yellow solid. This solid was recrystallized twice from ethyl acetate to afford 6.42 g of N-(2-(3,5-diaminobenzoyl)oxyethyl)-α-phenylmaleimide.