反応 #83397

反応方程式

meta-trifluoromethylphenol

sodium hydride

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

sodium hydride

→

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

溶媒

dimethylformamide

反応条件

後処理

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

実験手順

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.

出典