反応 #992702
ord-316ef3f7b4ed48edac9e493bced5fc41
反応方程式
反応物
試薬
反応条件
後処理
- 1温度The resulting mixture was heated
- 2温度at reflux for 3 days
- 3濃縮concentrated onto silica gel (0.5 g)
- 4その他The residue was purified by flash chromatography on silica gel
- 5洗浄eluted with 35% ethyl acetate in hexanes
実験手順
A solution of hydroxylamine hydrochloride (50 mg, 0.71 mmol) in water (0.5 mL) was added to a solution of 1-(3-chloro-2-pyridinyl)-N-[2-[(diethylamino)oxoacetyl]-4,6-dimethylphenyl]-3-(trifluoromethyl)-1H-pyrazole-5-carboxamide (i.e. the title product of Example 2, 124 mg, 0.24 mmol) in ethanol (5 mL) at 25° C. The resulting mixture was treated with a solution of sodium acetate (200 mg) in water (2 mL). The resulting mixture was heated at reflux for 3 days and then cooled to 25° C., diluted with ethanol (30 mL) and concentrated onto silica gel (0.5 g). The residue was purified by flash chromatography on silica gel eluted with 35% ethyl acetate in hexanes to give 50 mg of the title product, a compound of the present invention, as a yellow glassy solid.