反应详情

温度

80 °C

3-Amino-4,4,4-trichloro-2-cyano-N-(4-methoxy-3-pyridyl)but-2-enamide (37.2 g, 110.9 mmol) was dissolved in N-methylpyrrolidinone (200 mL). Hydrazine hydrate (14.43 g, 14.02 mL, 288.3 mmol) was added portionwise, then the mixture heated to 80° C. for 20 hr. The mixture was cooled to ambient and concentrated in vacuo. The viscous red oil was stirred as TBME (180 ml)/DCM (20 ml) was added. The yellow solid that precipitated was filtered, washed with TBME and dried to afford the title compound (26.9 g, 98%). LC-MS (M+H)+ 249.0; 1H NMR (500 MHz, DMSO-d6) δ 11.90 (br s, 1H), 9.32 (s, 1H), 9.14 (s, 1H), 8.15 (d, 1H), 7.10 (d, 1H), 3.92 (s, 3H).

1. temperatureThe mixture was cooled to ambient and
2. concentrationconcentrated in vacuo
3. additionwas added
4. filtrationThe yellow solid that precipitated was filtered
5. washwashed with TBME
6. customdried