反応 #736395

反応方程式

4-chloro-3-methoxy-2-methylpyridine

2,2,2-trifluoroethanol

potassium t-butoxide

→

3-methoxy-2-methyl-4-(2,2,2-trifluoroethoxy)pyridine

収率 46.8%

反応条件

後処理

1. 1
   濃縮concentrated
2. 2
   workup.ADDITIONdiluted with water
3. 3
   抽出extracted twice with chloroform
4. 4
   乾燥The extract was dried, from which chloroform
5. 5
   その他was evaporated
6. 6
   その他the residue was purified by column chromatography on silica gel (chloroform-methanol (400:9))

実験手順

A mixture of 4-chloro-3-methoxy-2-methylpyridine (7.8 g), 2,2,2-trifluoroethanol (24.7 g) and potassium t-butoxide (27.76 g) was heated at 110° C. for 18 hours, then concentrated, diluted with water, and extracted twice with chloroform. The extract was dried, from which chloroform was evaporated, and the residue was purified by column chromatography on silica gel (chloroform-methanol (400:9)), to give 3-methoxy-2-methyl-4-(2,2,2-trifluoroethoxy)pyridine (5.12 g) as a white or pale yellow solid.

出典