Sodium Hydroxide → HCID 178506296, compound

Temperature

0 °C

3.50 g of 3-(trifluoromethyl)-1H-pyrazole was suspended in 45 ml of water, and 3.2 g of 50% aqueous solution of sodium hydroxide was added to it. The mixture was cooled to 0° C., and then 3.20 g of bromine was added to the mixture, followed by stirring at room temperature for 7 hours. The reaction mixture was extracted by ethyl acetate. The organic layer was washed with water dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. Hexane was added to the residue, as a result, a crystal was formed. The crystal was collected to obtain 3.38 g of 4-bromo-3-(trifluoromethyl)-1H-pyrazole.

1. extractionThe reaction mixture was extracted by ethyl acetate
2. washThe organic layer was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. additionHexane was added to the residue, as a result
7. customa crystal was formed
8. customThe crystal was collected

ORD record

ord-58dc828c44e241b99546b12876d596e3

Source dataset

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07541374B2