反応 #65852

反応方程式

5-nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

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

nitric acid

→

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

溶媒

sulphuric acid

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度After cooling
3. 3
   抽出extracted with methylene chloride
4. 4
   洗浄After washing with sodium hydrogencarbonate solution
5. 5
   その他drying
6. 6
   濃縮the extract was concentrated on a rotary evaporator

実験手順

352 g of 5-nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 28 were taken and a mixture of 250 ml of 100% by weight nitric acid and 350 ml of concentrated sulphuric acid was added. The reaction mixture was stirred for 2 hours at 60° C. After cooling, it was poured into ice-water and extracted with methylene chloride. After washing with sodium hydrogencarbonate solution and drying, the extract was concentrated on a rotary evaporator. The yield was 392 g (91% of theory) and the melting point was 125° C. The NMR spectra showed the following characteristic absorptions: 19F NMR: -68.5 and -81.0 ppm. 1H NMR: 4.86 ppm.

出典