反应详情

温度

165 °C

The product of Example 320C (0.125 g, 0.29 mmol) was reacted with cesium carbonate (0.38 g, 1.17 mmol), 2-bromoacetamide (0.060 g, 0.43 mmol) and a catalytic amount of tetrabuylammonium iodide in N,N-dimethylformamide (3 mL) at 25° C. for 2 hours. The reaction was concentrated to half the volume under a stream of nitrogen warmed through a manifold heated to 165° C. The resulting solution was diluted with water and the precipitate was collected by filtration and dried to give the title compound (0.134 g, 95%). MS (ESI−) m/z 482 (M−H)−. The sodium salt of the title compound was prepared according to the procedure of Example 1D. 1H NMR (300 MHz, DMSO-d6) δ ppm 0.21 (m, J=3.86, 2.39 Hz, 2 H) 0.46 (m, 2 H) 0.99 (m, 1 H) 2.55 (m, 2 H) 4.49 (s, 2 H) 5.96 (t, J=6.43 Hz, 1 H) 7.06 (m, 1 H) 7.21 (m, 2 H) 7.40 (m, 2 H) 7.53 (m, 1 H) 7.62 (m, J=1.84 Hz, 1 H) 7.67 (d, J=8.46 Hz, 1 H) 8.07 (dd, J=8.09, 1.47 Hz, 1H) 16.25 (s, 1 H).

1. concentrationThe reaction was concentrated to half the volume under a stream of nitrogen
2. temperaturewarmed through a manifold
3. additionThe resulting solution was diluted with water
4. filtrationthe precipitate was collected by filtration
5. customdried