반응 #83397

반응 방정식

meta-trifluoromethylphenol

sodium hydride

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

sodium hydride

→

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

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
3. 3
   세척The obtained organic layer was washed with aqueous saturated sodium chloride
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   농축concentrated
6. 6
   기타purified on a silica gel column
7. 7
   기타to obtain the end product

실험 절차

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.

출처