反应详情

A 95% sulfuric acid (35 ml) was added to 2-chloro-4-fluorophenyl methanesulfonate (22.5 g), to which was then added dropwise a mixture of 95% sulfuric acid (7.5 ml) and 61% nitric acid (10.3 g) under ice-water cooling and stirring to effect nitration reaction. After the completion of the addition, the reaction mixture was stirred for further 30 minutes at room temperature and then poured onto ice pieces and extracted with toluene. The toluene extract as separated was washed with 1N aqueous sodium hydroxide solution and then with water and dried over anhydrous sodium sulfate. The toluene was distilled off to afford the titled compound (25.9 g) as pale yellow crystals with melting point 64°-65.5° C.

1. additionwas then added dropwise
2. customreaction
3. additionAfter the completion of the addition
4. stirringthe reaction mixture was stirred for further 30 minutes at room temperature
5. additionpoured onto ice pieces
6. extractionextracted with toluene
7. extractionThe toluene extract
8. customas separated
9. washwas washed with 1N aqueous sodium hydroxide solution
10. dry with materialwith water and dried over anhydrous sodium sulfate
11. distillationThe toluene was distilled off