반응 #65849

반응 방정식

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

nitric acid

sulphuric acid

→

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

용매

methylene chloride

반응 조건

후처리

1. 1
   기타the organic phase was separated off
2. 2
   추출the aqueous phase was extracted with methylene chloride
3. 3
   세척The combined organic phases were washed with water
4. 4
   기타dried
5. 5
   기타the readily volatile components were removed

실험 절차

A solution of 54.4 g of 2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole in 75 ml of methylene chloride was added dropwise at 10° C. to a mixture of 40 ml of 65% by weight nitric acid and 40 ml of concentrated sulphuric acid. The reaction mixture was subsequently stirred for 1 hour at room temperature and then poured into ice-water, the organic phase was separated off and the aqueous phase was extracted with methylene chloride. The combined organic phases were washed with water and dried and the readily volatile components were removed. The residue consisted of 95 g of product (=86% of theory) melting at 87° to 88° C. The NMR spectra showed the following characteristic absorptions: 19F NMR: -59.0 and -69.4 ppm. 1H NMR: 3.10 ppm.

출처