反应详情

温度

135 °C

A solution of 1-(2-fluoro-6-methoxyphenyl)ethanone (1 g), hydrazine (1.04 g), and sodium acetate (0.49 g) was stirred for 72 hours in toluene (10 mL). The mixture was concentrated, taken up in DMSO (8 mL), and heated to 135° C. for 24 hours. The mixture was cooled, poured into ethyl acetate (200 mL), and rinsed with 3× water, and brine. The organic layer was concentrated and chromatographed on silica gel using 10-100% ethyl acetate/hexanes.

1. concentrationThe mixture was concentrated
2. temperatureThe mixture was cooled
3. additionpoured into ethyl acetate (200 mL)
4. washrinsed with 3× water, and brine
5. concentrationThe organic layer was concentrated
6. customchromatographed on silica gel using 10-100% ethyl acetate/hexanes