PYRIDINE, 3-METHOXY-2-METHYL-4-(2,2,2-TRIFLUOROETHOXY)-, 1-OXIDE synthesis

Yield:-

Reaction Conditions:

with potassium tert-butylate in water;

Steps:

1.b b

b 2-Methyl-3-methoxy-4-(2,2,2-trifluoroethoxy)pyridine N-oxide 6.7 g of potassium tert-butoxide were added in portions, at -20° C., while stirring and under a nitrogen atmosphere, 5 to 20 ml of trifluoroethanol. After the mixture had been warmed to 0° C., 5.2 g (30 mmol) of 2-methyl-3-methoxy-4-chloropyridine N-oxide were added in portions. The mixture was heated under reflux for 3 hours, and then left to cool down to room temperature; a further 3.45 g of potassium tert-butoxide were then added and the mixture was heated under reflux for 2 hours. After it had cooled down, 40 ml of water were added to the reaction mixture, which was then extracted with dichloromethane; the extract was then dried over MgSO₄ and freed from the solvent in vacuo. The resulting oily product was subjected to further reaction.

References:

US5658933,1997,A