反应详情

317 g of the product of Example 27 were taken and a mixture of 250 ml of 100% by weight nitric acid and 350 ml of concentrated sulphuric acid was added dropwise, with stirring. The reaction mixture was stirred for 2 hours at 55° C. It was then left to cool and poured into ice-water. The product was extracted with methylene chloride, the extract was washed with sodium hydrogen-carbonate solution until the washings were neutral, and dried, and the readily volatile components were removed on a rotary evaporator. The yield was 339 g (=94% of theory) and the melting point was 101° to 103° C. The NMR spectra showed the following characteristic absorptions: 19F NMR: -60.9 and -86.5 ppm. 1H NMR: 3.18 ppm.

1. additionwas added dropwise
2. stirringThe reaction mixture was stirred for 2 hours at 55° C
3. waitIt was then left
4. temperatureto cool
5. extractionThe product was extracted with methylene chloride
6. washthe extract was washed with sodium hydrogen-carbonate solution until the washings
7. customdried
8. customthe readily volatile components were removed on a rotary evaporator