ethyl 4-(4-cyanophenyl)-2,4-dioxobutanoate synthesis

Yield:649557-55-1 74%

Reaction Conditions:

with sodium ethanolate in ethanol at 20; for 4 h;

Steps:

Ethyl [4- (4-CYANOPHENYL)-2,] 4-dioxobutanoate To a solution of the available 4-acetylbenzonitrile (5.0 g, 0.034 mol) in EtOH (100 [ML) WAS ADDED THE SODIUM ETHYLAT (2.8 G, 1.2 EQ. ) AND THE REACTION WAS STIRRED TO RT DURING 1 HOUR. THEN, DIETHYL OXALATE (4.7 ML, 1.0 EQ. ) WAS ADDED AND THE REACTION] was stirred at rt for 3 hours. After concentration, the mixture was diluted in [ET20.] The formed precipitate was filtered, washed with [ET20] and dried to give the title compound as a pink solid (6.21 g, 0.025 mol) in a 74% yield ; LC/MS: M+H [C13HL2NO4] 246

References:

WO2004/6922,2004,A1 Location in patent:Page/Page column 49