Hydrochloric Acid → 5-Chloro-2-nitro-4-(trifluoromethyl)phenol

Temperature

80 °C

A mixture of 10 g of 2,4-dichloro-5-nitrobenzotrifluoride, 4.15 g of potassium acetate and 60 ml of DMF was stirred while heating at 60° C. for one hour and at 80° C. for three hours. To the reaction mixture, 4.15 g of potassium acetate was added. The reaction mixture was stirred while heating at 80° C. for further one hour. The reaction mixture was cooled to room temperature, and 1 M hydrochloric acid was added thereto, followed by extraction with ethyl acetate. The combined organic layers were washed with water and a saturated sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 7.55 g of 5-chloro-2-nitro-4-trifluoromethylphenol.

1. stirringThe reaction mixture was stirred
2. temperaturewhile heating at 80° C. for further one hour
3. temperatureThe reaction mixture was cooled to room temperature
4. extractionfollowed by extraction with ethyl acetate
5. washThe combined organic layers were washed with water
6. dry with materiala saturated sodium chloride solution, dried over magnesium sulfate
7. concentrationconcentrated under reduced pressure

ORD record

ord-06e17b1b468e46eda103456b226a56a4

Source dataset

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08445522B2