반응 #898

반응 방정식

m-(Trifluoromethyl)phenol

NaH

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

→

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

용매

THF

반응 조건

후처리

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

실험 절차

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.

출처