4-Nitrophenol → 1-(2-Bromo-1,1,2-trifluoroethoxy)-4-nitrobenzene

Temperatur

40 °C

278 g of 4-nitrophenol and 56 g of potassium hydroxide were dissolved in 800 ml of dimethylformamide, 179 g of bromotrifluoroethylene were fed in, a little at a time, at 40° C., and stirring was then continued for 2 hours at 60° C. The solvent was removed under reduced pressure in a rotary evaporator, the residue was poured into ice-water and extracted with 3×500 ml of methylene chloride, the extract was washed with dilute sodium hydroxide solution and water and dried over Na2SO4, and the solvent was removed. When the residue was distilled, 279.5 g of pure product passed over at 114° C./1.3 mbar.

1. customThe solvent was removed under reduced pressure in a rotary evaporator
2. additionthe residue was poured into ice-water
3. extractionextracted with 3×500 ml of methylene chloride
4. washthe extract was washed with dilute sodium hydroxide solution and water
5. dry with materialdried over Na2SO4
6. customthe solvent was removed
7. distillationWhen the residue was distilled
8. custompassed over at 114° C./1.3 mbar

ORD-Eintrag

ord-9743f657a1bb436fa06a197d84f451d0

Quelldatensatz

uspto-grants-1985_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04551448