Dimethoxyphenyl-2-propanone from 3,4-Dimethoxy-l,2-dihydroxypropane

One portion (61 parts) of the glycol product was distilled slowly under vacuum (5 mms Hg) in the presence of 0.5% by weight of anhydrous zinc chloride. The product (37 parts) had a boiling point of 155 to 160° C. 15 mm Hg and was crude 3,4-dimethoxyphenylacetone. 

A second portion (50 parts) was refluxed with dilute sulphuric acid (250 parts of 4% acid) for two hours. The reaction, mixture was extracted with ether and the extracted ketone recovered by removal of the solvent from the extract. The oily ketone product had a boiling point of 142 to 150°C/3 mms Hg. Source Bush 1968 

A standard experimental procedure was followed in the examples. When the experimental conditions deviated from standard procedure, it is noted in the description of the experiment. 

Benzyl chloride (126.6 grams (1 mole)) was dissolved in the tetrahydrofnran. The reaction started at 73° C and was maintained between 77° C and 80° C. The reaction was completed in 1 hour and 16 minutes. The yield of benzyl magnesium chloride complex as titrated was 49% magnesium consumed, 69.2% 

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