Reacción #898

Ecuación de reacción

m-(Trifluoromethyl)phenol

NaH

4-chloro-2-methylthio-6-(trifluoromethyl)pyrimidine

→

2-methylthio-4-trifluoromethyl-6-[3-(trifluoromethyl)phenoxy]pyrimidine

Disolventes

THF

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONVII-17) (1.0 g, 0.0044 mol) was added
2. 2
   TemperaturaThe resulting solution was refluxed for about 7 hours
3. 3
   OtroThe reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
4. 4
   Otroto separate an organic phase
5. 5
   LavadoThe organic phase was washed with aqueous saturated sodium chloride
6. 6
   Secadodried over anhydrous sodium sulfate
7. 7
   Concentraciónconcentrated
8. 8
   workup.DISTILLATIONwere distilled off in a tubular oven (under water flow, 150° C.)
9. 9
   Otroto obtain the intermediate compound

Procedimiento

m-(Trifluoromethyl)phenol (1.06 g, 0.0044×1.5 mol) and NaH (0.26 g (ca.60% in mineral oil), 0.0044×1.5 mol) were dissolved in THF, and then 4-chloro-2-methylthio-6-(trifluoromethyl)pyrimidine (Compound No. VII-17) (1.0 g, 0.0044 mol) was added thereto. The resulting solution was refluxed for about 7 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate to separate an organic phase. The organic phase was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated. Thereafter, remaining phenol and others were distilled off in a tubular oven (under water flow, 150° C.) to obtain the intermediate compound.

Fuente