反应详情

温度

90 °C

To a solution of the acid of Example 16 (0.72 g, 1.52 mmol), in benzene (25 mL) is added triethylamine (0.23 mL, 1.1 equiv) followed by diphenylphosphoryl azide (0.46 g, 1.1 equiv). After the reaction mixture is heated at 90° C. for 1 hour, a solution of hydroxylamine hydrochloride (0.23 g, 2.2 equiv.) in a mixture of triethylamine (0.46 mL) and water (0.25 mL) is added to it, and the reaction mixture is heated at 90° C. overnight. The reaction is quenched by addition of ammonium chloride solution, and the resulting precipitate is filtered off, washed with water and ethyl acetate and dried to afford 0.45 g (59%) of a white solid, m.p. 184°-186° C.

1. additionis added to it
2. temperaturethe reaction mixture is heated at 90° C. overnight
3. customThe reaction is quenched by addition of ammonium chloride solution
4. filtrationthe resulting precipitate is filtered off
5. washwashed with water and ethyl acetate
6. customdried