反应详情

温度

250 °C

To a stirred solution of DOWTHERM (300 mL) at 250° C. was added a solution of the product of Step 2 (30.0 g, 87 mmol) in DOWTHERM (30 mL). The resulting solution was stirred at 250° C. for 5 minutes, cooled to RT and filtered. The resulting cake was washed with hexane (3×50 mL), then dried to give the title product. 1H NMR (400 MHz, CD3OD) δ 8.25 (s, 1H); 6.92 (s, 1H); 5.80 (s, 1H); 4.27 (q, J=7.1 Hz, 2H); 3.97 (s, 3H); 1.46 (t, J=7.0 Hz, 3H) ppm. LRMS (ESI) m/z 298.0 [(M+H)+; calcd for C12H13BrNO3: 298.0].

1. temperaturecooled to RT
2. filtrationfiltered
3. washThe resulting cake was washed with hexane (3×50 mL)
4. customdried