反应详情

To a solution of 3-phenylisoxazole-5-carboxylic acid (1.0 g, 5 mmol, 1.0 equiv.) in DMF (20 mL) and THF (20 mL), was added HBTU (2.28 g, 6 mmol, 1.2 equiv.), followed by sodium azide (0.65 g, 10 mmol, 2.0 equiv.) and DIEA (2.6 mL, 15 mmol, 3.0 equiv.). The mixture was stirred at RT for 30 min, concentrated, followed by adding of H2O (40 mL). The precipitate was filtered, washed with H2O, and dried in vacuo to give 3-phenylisoxazole-5-carbonyl azide (0.65 g, 60%). LRMS (M−18+H+) m/z 187.1.

1. concentrationconcentrated
2. additionby adding of H2O (40 mL)
3. filtrationThe precipitate was filtered
4. washwashed with H2O
5. customdried in vacuo