Sodium 1-oxidopyridin-1-ium-2-thiolate → 2-[1-(2,6-Difluorophenyl)ethylthio]pyridine 1-oxide

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

2,6-Difluoro-alpha-methylbenzyl chloride (16.6 g, 0.094 mol) is dissolved in ethanol (40 ml) and warmed to 75° C. A 40 percent solution of sodium omadine (38.5 g, 0.103 mol) is added dropwise over a period of 30 minutes maintaining a reaction temperature of 75° C. throughout. Once the addition is complete, the reaction mixture is kept between 75° C. and 80° C. for 2 hours. Thereafter the mixture is quenched in ice-water and crude product is filtered off. After recrystallization with ethyl acetate pure title product (10.65 g, 42.4%) is obtained; Melting Point 158°-160° C.

Herkunft & Nachweise