| 摘要 |
Preparation of substituted trans cinnamaldehyde compounds (I) comprises oxidizing substituted phenylpropane derivatives in a solvent in the presence of catalyst and oxidant. Mother liquor is then separated from the mixture and a residue is formed which is dissolved in an organic solvent. The organic layer is separated, dried and evaporated to form a residue that is purified. Preparation of substituted trans-cinnamaldehyde (I) comprises: (1) oxidizing substituted phenylpropane derivatives (II) in a solvent in the presence of the catalyst and an oxidizing agent at -15 deg C to 210 deg C for 0.5-48 hours; (2) cooling the resulting mixture and filtering unwanted solid and separating clear mother liquor; (3) removing solvent from the mother liquor under reduced pressure to yield a residue; (4) forming a solution of the residue in an organic solvent, washing residue optionally with aqueous alkali solutions, followed by brine solution and separating organic layer and discarding aqueous layer, and (5) drying the organic layer over anhydrous sodium sulfate, filtering and evaporating the organic layer to obtain another residue which is purified by column chromatography over silica gel to obtain (I) (68-72%). R1 = CH=CH-CHO, and R2-R6 = H, alkoxy containing at least two H atoms or one methylene dioxy group, at least one methylenedioxy, at least a OH and H, or at least a protected OH such as acetyl, benzyl or H with a combination of the remaining substituents comprising alkoxy, OH, methylenedioxy, 1-2C alkyl, aryl or H. |
