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0 °C

1-(4-fluorophenyl)-2-(5-(trifluoromethyl)pyridin-2-yl)ethanone oxime. To a solution of 1-(4-fluorophenyl)-2-(5-(trifluoromethyl)pyridin-2-yl)ethanone (8.00 g, 28.2 mmol) in methanol (100 ml) at room temperature was added 15% NaOH (29 ml, 109 mmol). The resulting solution was stirred vigorously as solid hydroxylamine hydrochloride (9.8 g, 140 mmol) was added portionwise. The mixture was heated to reflux for 1 hour, treated with charcoal while hot, and then quickly filtered through Celite before being allowed to cool. The filtrate was concentrated to one-half of its original volume and then cooled to 0° C. for 1 hour. The resultant solids were collected by filtration, washed with water, and dried under vacuum at 50° C. overnight to provide 5.00 g (59%) of the title compound as a dark yellow solid.

1. additionwas added portionwise
2. temperatureThe mixture was heated
3. temperatureto reflux for 1 hour
4. filtrationthen quickly filtered through Celite
5. temperatureto cool
6. concentrationThe filtrate was concentrated to one-half of its original volume
7. filtrationThe resultant solids were collected by filtration
8. washwashed with water
9. customdried under vacuum at 50° C. overnight