反应详情

温度

150 °C

A stirred solution of N2-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-4-[(2,2,2-trifluoroethyl)oxy]-1,2-benzenediamine (D57, 95 mg, 0.25 mmol) in tetrahydrofuran (5 ml) at room temperature under argon was treated with N,N-diisopropylethylamine (100 mg, 0.78 mmol) followed by ethyl chloroformate (33 mg, 0.30 mmol) and maintained for 3 days. The mixture was concentrated under vacuum and the residue treated with dimethylformamide (5 ml) and heated at 150° C. under argon for 7 hrs. The solution was concentrated under vacuum and the residue treated with 10% Na2CO3 solution and extracted with ethyl acetate. The extract was dried (Na2SO4) and concentrated under vacuum to leave a brown oil, which was purified by Mass-Directed Automated HPLC to afford the title compound as a white solid. This was converted to its HCl salt and isolated as a beige solid (30 mg, 29%).

1. temperaturemaintained for 3 days
2. concentrationThe mixture was concentrated under vacuum
3. additionthe residue treated with dimethylformamide (5 ml)
4. concentrationThe solution was concentrated under vacuum
5. additionthe residue treated with 10% Na2CO3 solution
6. extractionextracted with ethyl acetate
7. dry with materialThe extract was dried (Na2SO4)
8. concentrationconcentrated under vacuum
9. customto leave a brown oil, which
10. customwas purified by Mass-Directed Automated HPLC