反应详情

温度

0 °C

A solution of 3-hydroxymethyl-5-trifluoromethyl-benzonitrile (200 mg, 0.994 mmol) in toluene (1 ml) at 0° C. was treated with diphenyl phosphoryl azide (328 mg, 1.19 mmol), followed by DBU (182 mg, 1.19 mmol) and stirred at 0° C. for 2 hours. The ice bath was removed and the reaction was stirred at room temperature for overnight. Reaction was diluted with ethyl acetate and washed with 10% HCl solution, dried over anhydrous magnesium sulphate and concentrated in vacuo. The residue was purified by silica gel chromatography over 12+S Biotage silica column (eluted with 0-30% ethyl acetate in hexanes) to yield the title compound (150 mg, 67%) as a colorless oil. 1H NMR (400 MHz, CDCl3) δ ppm 4.54 (s, 2H) 7.82 (s, 2H) 7.88 (s, 1H).

1. customThe ice bath was removed
2. stirringthe reaction was stirred at room temperature for overnight
3. customReaction
4. washwashed with 10% HCl solution
5. dry with materialdried over anhydrous magnesium sulphate
6. concentrationconcentrated in vacuo
7. customThe residue was purified by silica gel chromatography over 12+S Biotage silica column (eluted with 0-30% ethyl acetate in hexanes)