反应详情

温度

250 °C

A solution of ethyl (3E)-3-[(4-bromo-3-methoxyphenyl)imino]-3-ethoxypropanoate (30.0 g, 87 mmol) in DOWTHERM (30 mL) was added to a stirred solution of DOWTHERM (300 mL) at 250° C. The resulting solution was stirred at 250° C. for 5 minutes, cooled to RT and filtered, and the 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 cake was washed with hexane (3×50 mL)
4. customdried