反应详情

温度

105 °C

To a stirred suspension of the title compound of Example 1, Step G (3.3 g, 8 mmol) in 25 mL toluene and 0.02 g DMF was added at 80° C. thionyl chloride (1.31 g, 11 mmol) over a period of 15 minutes. The suspension was stirred at the same temperature for 2 h and at 105° C. for 30 minutes. After cooling to room temperature, the organic layer was washed with water, dried, and the solvent was evaporated under reduced pressure to yield the title compound of Step A, a compound of this invention, in quantitative yield as a crude powdery product melting at 169-170° C. 1H NMR (CDCl3) δ 7.64 (d, 1H), 7.36 (d, 1H), 7.20 (br s, 1H), 4.78 (m, 2H), 4.56 (s, 2H), 4.24 (dd, 1H), 3.62 (dd, 1H), 2.62 (m, 1H), 2.38 (m, 1H).

1. temperatureAfter cooling to room temperature
2. washthe organic layer was washed with water
3. customdried
4. customthe solvent was evaporated under reduced pressure