反応 #896

反応方程式

NaH

4-chloro-2-(methylthio)pyrimidine

3-(trifluoromethyl)phenol

→

phenoxide

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

溶媒

THF

反応条件

後処理

1. 1
   workup.ADDITIONVII-1) (3.0 g, 0.0187 mol) was added
2. 2
   温度the mixture was refluxed for about 10 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
   その他recrystallized from a methanol/water system
9. 9
   その他to obtain the intermediate compound

実験手順

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.

出典