تفاعل #898

معادلة التفاعل

m-(Trifluoromethyl)phenol

NaH

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

→

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

المذيبات

THF

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر