Nitric Acid → HCID 178526653, compound

Temperature

80 °C

To a mixture of 9.84 g of 2-hydroxy-5-(trifluoromethyl)pyridine and 40 ml of concentrated sulfuric acid, 10.9 g of 70% nitric acid was dropped at 80° C. This mixture was stirred at 80° C. for 1 hour. The reaction mixture was cooled down to room temperature, then, the reaction mixture was poured into ice water. The deposited solid was collected by filtration. This solid was washed with ice water, then, dissolved in ethyl acetate, and washed with saturated saline. The organic layer was dried over magnesium sulfate, then, concentrated under reduced pressure, to obtain 5.22 g of 2-hydroxy-3-nitro-5-(trifluoromethyl)pyridine.

1. additionwas dropped at 80° C
2. temperatureThe reaction mixture was cooled down to room temperature
3. filtrationThe deposited solid was collected by filtration
4. washThis solid was washed with ice water
5. dissolutiondissolved in ethyl acetate
6. washwashed with saturated saline
7. dry with materialThe organic layer was dried over magnesium sulfate
8. concentrationconcentrated under reduced pressure

ORD record

ord-e806b37e01d5444b951507f70ffb56fd

Source dataset

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08742112B2