反应详情

温度

-78 °C

2-[(1-Azabicyclo[3.3.0]octan-5-yl)ethylamino]benzonitrile (1.34 g, 5.25 mmol) obtained by Example 27 was mixed with concentrated sulfuric acid (48.2 ml) and water 7.5 ml to react the mixture for 2 hours at 110° C. The reaction mixture was cooled to -78° C., neutralized by 25% ammonia solution, extracted by ethyl acetate, washed by water, dried over anhydrous sodium sulfate, concentrated in vacuo, and crystallized from ethyl acetate to afford the desired compound (961 mg, 67.0%).

1. customto react the mixture for 2 hours at 110° C
2. extractionextracted by ethyl acetate
3. washwashed by water
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. customcrystallized from ethyl acetate