89976-12-5

13630-19-8

89976-12-5

General procedure for the synthesis of 2-methyl-5-nitrobenzotrifluoride from o-toluotrifluoride: 50 g of 2-trifluoromethyltoluene and 250 g of 98% sulfuric acid were added to a 250 mL four-necked flask with stirring and cooled to 10°C. The reaction was carried out over a period of time. 50 g of 65% nitric acid was added slowly and dropwise over a period of about 2 hours to ensure complete reaction. Upon completion of the reaction, the reaction solution was poured into 200 g of crushed ice and layered with 150 mL of dichloromethane. The aqueous phase was extracted once more with 100 mL of dichloromethane and the organic phases were combined. The organic phase was washed sequentially with 80 mL of saturated sodium bicarbonate solution and 50 mL of water. Concentration to dryness gave 62 g of a light yellow oily product in 97% yield. The product did not need further purification and could be used directly in the next reaction.