3,5-Dimethylanisole was dispersed in 1 mL of iso-octane and slowly added dropwise over 20 minutes to a pre-prepared 3,5-dimethylanisole/iso-octane/TiCl4 mixed system. Sticky material was observed to precipitate during the reaction, and the reaction system was kept at -15 °C with continuous stirring for 4.5 hours. Upon completion of the reaction, the reaction was quenched with water and subsequently treated with NaOH solution. Subsequent operations were performed with reference to the standard post-treatment process of Example 1. Analysis of the product mixture by gas chromatography (GC) showed that it contained about 40% unreacted 3,5-dimethylanisole and about 53% of the target product, a mixture of 2-methoxy-4,6-dimethylbenzaldehyde and 4-methoxy-2,6-dimethylbenzaldehyde, in a total yield of about 53%.
