تفاعل #896

معادلة التفاعل

NaH

4-chloro-2-(methylthio)pyrimidine

3-(trifluoromethyl)phenol

→

phenoxide

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

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONVII-1) (3.0 g, 0.0187 mol) was added
2. 2
   درجة الحرارةthe mixture was refluxed for about 10 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
   أخرىrecrystallized from a methanol/water system
9. 9
   أخرىto obtain the intermediate compound

الإجراء التجريبي

In THF, a phenoxide was prepared from 3-(trifluoromethyl)phenol (4.54 g, 0.0187×1.5 mol) was mixed with NaH (1.12 g (ca. 60% in mineral oil), 0.0187×1.5 mol), and 4-chloro-2-(methylthio)pyrimidine (Compound No. VII-1) (3.0 g, 0.0187 mol) was added thereto and the mixture was refluxed for about 10 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, then recrystallized from a methanol/water system to obtain the intermediate compound.

المصدر