Trimethyl orthoformate → 1-(1,1-Dimethoxyethyl)-2,4-difluorobenzene

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Reaction Steps

In a solution composed of 15.7 g of 2,4-difluoroacetophenone, 35 g of trimethyl ortho-formate and 15 g of methanol, 0.96g of p-toluenesulfonic acid was added, and reacted at 40° C. to 45° C. for 2 hours. This was added to an aqueous solution of 5% by mass sodium hydrogen carbonate, which was then extracted with ethyl acetate. An extract was washed with water, and dried on Na2SO4. Then, ethyl acetate was concentrated to yield 18.2 g of 1-(1,1-dimethoxyethyl)-2,4-difluorobenzene. It was confirmed that the 1-(1,1-dimethoxyethyl)-2,4-difluorobenzene had NMR data of (CDCl3, δppm) 1.62 (s, 3H), 3.9 (s, 6H), 6.74-6.9 (m, 2H), 7.56-7.7 (m, 1H) by NMR (supplied from Varian Technologies Japan Limited).

Provenance & Evidence