反应详情

温度

80 °C

Sodium azide (1.51 g, 23.2 mmol) was added to a suspension of 4-(4-bromo-2-chlorophenylamino)-6-chloronicotinic acid tert-butyl ester (40) (3.23 g, 7.73 mmol) in DMF (60 mL). The reaction mixture was heated to 80° C. and stirred for 16 hours. After cooling to room temperature, the reaction was diluted with EtOAc and washed with water, saturated NaHCO3 and brine. The organic layer was dried (Na2SO4) and concentrated. Purification by flash column chromatography using the Biotage system (CH2Cl2) (repeated) provided the desired product (41) (1.41 g, 43%).

1. temperatureAfter cooling to room temperature
2. washwashed with water, saturated NaHCO3 and brine
3. dry with materialThe organic layer was dried (Na2SO4)
4. concentrationconcentrated
5. customPurification by flash column chromatography