反应详情

温度

90 °C

In a 50 mL pear-shaped flask, ethyl 3-(4-bromo-2-fluorophenyl)propiolate (1.27 g, 4.68 mmol) and (azidomethyl)trimethylsilane (2.42 g, 2.78 mL, 18.7 mmol, Eq: 4) were combined with benzene (3.5 mL) to give a light yellow solution. The reaction mixture was heated to 90° C. and stirred for 4 h. The reaction mixture was concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 80 g, 0% to 20% EtOAc in heptane) to afford 616 mg (33%) of the desired less polar regio-isomer as a white solid. (M+H)+=400.0/402.0 m/e.

1. customto give a light yellow solution
2. concentrationThe reaction mixture was concentrated in vacuo
3. customThe crude material was purified by flash chromatography (silica gel, 80 g, 0% to 20% EtOAc in heptane)
4. customto afford 616 mg (33%) of the