反应详情

温度

65 °C

To a solution of 5-Bromo-4-(2,2,2-trifluoro-ethoxy)-pyridine-2-carboxylic acid (methyl-cyano-cyclopropyl-methyl)-amide (Example 78e, 900 mg, 2.29 mmol) in ethanol (15 ml) were added triethylamine (244 mg, 336 μl, 2.41 mmol) and hydroxylamine hydrochloride (167 mg, 2.41 mmol). The reaction mixture was then stirred at 65° C. for 18 hours. Volatiles were removed in vacuo and the residue was dissolved in ethylacetate which was extracted with an 1.0M aqueous solution of sodium bicarbonate. The organic phase was dried over sodium sulfate and evaporated down to dryness. The crude material was purified by flash chromatography on silica eluting with a heptane/ethylacetate gradient to yield the title compound (576 mg, 59%) as a white solid. MS (ESI, m/z): 425.3 (M+H+).

1. customVolatiles were removed in vacuo
2. dissolutionthe residue was dissolved in ethylacetate which
3. extractionwas extracted with an 1.0M aqueous solution of sodium bicarbonate
4. dry with materialThe organic phase was dried over sodium sulfate
5. customevaporated down to dryness
6. customThe crude material was purified by flash chromatography on silica eluting with a heptane/ethylacetate gradient