反应详情

To a solution of 63.2 g (0.20 mole) of 4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid in 160 ml of concentrated sulfuric acid is added 40 ml of fuming nitric acid (90%) dropwise with stirring at 0°-5°. Following the nitric acid addition the solution is allowed to warm to 20° with stirring over a 1-hour period. The solutionis then added to a mixture of ice and water and allowed to stand for 18 hours. A precipitate results and is filtered, washed with water and dissolved in ether to obtain a solution which is washed with water, dried with anhydrous magnesium sulfate, filtered, and evaporated to give a residual solid. The residual solid is recrystallized from chlorobutane to give 40 g of 2-nitro-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid having a melting point of 115°-116°.

1. temperatureto warm to 20°
2. stirringwith stirring over a 1-hour period
3. customA precipitate results
4. filtrationis filtered
5. washwashed with water
6. dissolutiondissolved in ether
7. customto obtain a solution which
8. washis washed with water
9. dry with materialdried with anhydrous magnesium sulfate
10. filtrationfiltered
11. customevaporated
12. customto give a residual solid
13. customThe residual solid is recrystallized from chlorobutane