反应 #896

反应方程式

NaH

4-chloro-2-(methylthio)pyrimidine

3-(trifluoromethyl)phenol

→

phenoxide

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

溶剂

THF

反应条件

后处理

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
   其他The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
4. 4
   其他to separate an organic phase
5. 5
   洗涤The organic phase was washed with aqueous saturated sodium chloride
6. 6
   干燥dried over anhydrous sodium sulfate
7. 7
   浓缩concentrated
8. 8
   其他recrystallized from a methanol/water system
9. 9
   其他to obtain the intermediate compound

实验过程

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.

来源