反应 #83397

反应方程式

meta-trifluoromethylphenol

sodium hydride

2-chloro-6-(2-thienylmethyloxy)pyridine

sodium hydride

→

2-(2-thienylmethyloxy)-6-(meta-trifluoromethylphenoxy)pyridine

溶剂

dimethylformamide

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   其他the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
3. 3
   洗涤The obtained organic layer was washed with aqueous saturated sodium chloride
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   浓缩concentrated
6. 6
   其他purified on a silica gel column
7. 7
   其他to obtain the end product

实验过程

To a solution containing meta-trifluoromethylphenol (3.62 g, 0.0045×5.0 mol), sodium hydride (0.36 g, (Ca.60% in mineral oil), 0.0045×2.0 mol) and CuI (0.42 g, 0.0045×0.5 mol) in dimethylformamide, 2-chloro-6-(2-thienylmethyloxy)pyridine (1.0 g, 0.0045 mol) was added and the resultant solution was refluxed for about 3 hours. Additional sodium hydride (0.36 g, (60% in mineral oil), 0.0045×2.0 mol) was added thereto and the resultant solution was refluxed for another about 1 hour, thereafter the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The obtained organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and thereafter, concentrated and purified on a silica gel column to obtain the end product.

来源