반응 #65851

반응 방정식

product

5-Nitro-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

nitric acid

→

5,6-Dinitro-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

용매

sulphuric acid

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   workup.STIRRINGThe reaction mixture was stirred for 2 hours at 55° C
3. 3
   workup.WAITIt was then left
4. 4
   온도to cool
5. 5
   추출The product was extracted with methylene chloride
6. 6
   세척the extract was washed with sodium hydrogen-carbonate solution until the washings
7. 7
   기타dried
8. 8
   기타the readily volatile components were removed on a rotary evaporator

실험 절차

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.

출처