Potassium Carbonate → (4-Chlorophenyl)[3-chloro-5-(trifluoromethyl)-2-pyridinyl]methanone

Temperatur

23 °C

A solution of 2.0 g of 3-chloro-2-[1-(4-chlorophenyl)-1-cyanomethyl]-5-trifluoromethylpyridine (prepared by the method of Example 1) in 20 ml of dimethyl sulfoxide was admixed with a solution of 2.0 g of potassium carbonate in 3 ml of water, and the mixture was then stirred at 23° C. for 3 days under air. For work-up, the reaction mixture was poured into 200 ml of water. The product of value was then extracted with tert-butyl methyl ether (three times 80 ml). The combined organic phases were washed with water (two times 50 ml each), dried over sodium sulfate and finally concentrated. The resulting black oil was purified by Kugelrohr distillation under reduced pressure. Yield: 1.2 g (62%) of a light-yellow oil; boiling range: 110-120° C. (0.3 mbar); 1H NMR see Ex. 7.

1. extractionThe product of value was then extracted with tert-butyl methyl ether (three times 80 ml)
2. washThe combined organic phases were washed with water (two times 50 ml each)
3. dry with materialdried over sodium sulfate
4. concentrationfinally concentrated
5. distillationThe resulting black oil was purified by Kugelrohr distillation under reduced pressure

ORD-Eintrag

ord-ece2c5a3ad7245489279235f9417cc59

Quelldatensatz

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06337305B1