[OH-].[Na+].[C:3]([CH2:5][C:6]([O:8]C)=[O:7])#[N:4].[CH3:10][N:11]([CH3:20])[C:12]1[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=1.Cl>C(O)C>[C:3]([C:5](=[CH:16][C:15]1[CH:18]=[CH:19][C:12]([N:11]([CH3:20])[CH3:10])=[CH:13][CH:14]=1)[C:6]([OH:8])=[O:7])#[N:4]In 400 ml of an aqueous solution of 13.77 g of sodium hydroxide, 34.80 g of methyl cyanoacetate was dissolved and 34.01 g of p-dimethylamino benzaldehyde was then added under a nitrogen atmosphere, followed by adding 200 ml of ethanol to obtain a uniform solution. Under reflux, the stirring was continued for 51 hours and the reaction mixture was added to 12 N hydrochloric acid to obtain the precipitates. The resultant solid was repeated twice to recrystallize from a methanol/ethanol mixture to obtain 13.51 g of the needles.
読み込み中…
