反应详情

温度

40 °C

About 500 parts of aqueous nitric acid was added slowly, with stirring, to a reaction vessel containing about 400 parts of 3-chloro-4-fluorobenzotrifluoride. The temperature of the reaction mixture was maintained at about 40° C. during the addition, then raised to about 60° C. and maintained thereat for about 5 hours. The reaction mixture was allowed to settle. The aqueous layer was removed and the organic layer was washed twice with 500 parts of water, treated several times with a saturated solution of sodium bicarbonate, washed with water again, dried over anhydrous magnesium sulfate, and filtered. The filtrate was distilled at reduced pressure to yield 347 parts of 5-chloro-4-fluoro-2-nitrobenzotrifluoride.

1. temperatureraised to about 60° C.
2. temperaturemaintained
3. customThe aqueous layer was removed
4. washthe organic layer was washed twice with 500 parts of water
5. additiontreated several times with a saturated solution of sodium bicarbonate
6. washwashed with water again
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. distillationThe filtrate was distilled at reduced pressure