反应详情

9 g of 3-fluorophthalic anhydride and 6.8 g of malonic acid are mixed in 80 ml of triethylamine and heated in an oil bath at 71-72° until evolution of gas ceases. The reaction mixture is mixed with 50 ml of 10% HCl/H2O and extracted with ether. The ether is evaporated off and the resulting black oil chromatographed on a column using 1 l of 20% of ethylacetate/hexane followed by 1 l of 30% ethylacetate/hexane to yield first the 3fluoro-isomer followed by the desired 6-fluoro isomer; m.p. 76-81.5°.

1. temperatureheated in an oil bath at 71-72° until evolution of gas ceases
2. extractionextracted with ether
3. customThe ether is evaporated off
4. customthe resulting black oil chromatographed on a column
5. customto yield first the 3fluoro-isomer