反応 #898

反応方程式

m-(Trifluoromethyl)phenol

NaH

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

→

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

溶媒

THF

反応条件

後処理

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

実験手順

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.

出典