Phenylphosphonic dichloride → 5-Bromo-2-chloro-3-(trifluoromethyl)pyridine

Temperature

135 °C

The product of Example 5 (11.5 g, 0.048 mol) and phenylphosphoryl dichloride (45 mL) were heated with stirring at 135° C. for four hours and allowed to cool to room temperature. The reaction mixture was poured onto ice (750 g) and allowed to warm to room temperature. The mixture was extracted with dichloromethane (150 mL) and filtered. The organic phase was separated, washed with water and 10% sodium carbonate solution and dried over anhydrous sodium sulphate. Evaporation of the solvent gave 2-chloro-3-trifluoromethyl-5-bromopyridine (11.6 g) as a yellow oil.

1. temperatureto cool to room temperature
2. additionThe reaction mixture was poured onto ice (750 g)
3. temperatureto warm to room temperature
4. extractionThe mixture was extracted with dichloromethane (150 mL)
5. filtrationfiltered
6. customThe organic phase was separated
7. washwashed with water and 10% sodium carbonate solution
8. dry with materialdried over anhydrous sodium sulphate
9. customEvaporation of the solvent

ORD record

ord-bc1178f62f794614881bac365465cca1

Source dataset

uspto-grants-1999_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05968875