反应详情

温度

75 °C

To methyl 5-[3-({1-[2-(benzyloxy)phenyl]cyclopropyl}amino)-5-bromo-2-oxopyrazin-1(2H)-yl]-2-fluoro-4-methylbenzoate (Example 318e, 2.310 g) in ethanol (30 mL) was added ammonium formate (3.53 g) and Pd/C (0.042 g). The reaction was heated at 75° C. for 3 h. Hunig's Base (3 mL) was added, and the reaction was heated at 90° C. for 4 h. Additional catalyst, ammonium formate and hunigs base were added, and the reaction was heated at 90° C. for 4 h. The reaction mixture was then filtered warm, through a fibre glass filter, washing through with 500 mL ethanol, followed by 500 mL DCM, followed by 500 mL 10% methanol/DCM. The DCM and MeOH/DCM filtrates were combined, evaporated, and the resulting residue partitioned between DCM and water. The organic layer was separated, dried (MgSO4), filtered, and evaporated to give the subtitle compound as a solid (1.063 g).

1. temperaturethe reaction was heated at 90° C. for 4 h
2. temperaturethe reaction was heated at 90° C. for 4 h
3. filtrationThe reaction mixture was then filtered
4. temperaturewarm, through a fibre glass
5. filtrationfilter
6. washwashing through with 500 mL ethanol
7. customevaporated
8. customthe resulting residue partitioned between DCM and water
9. customThe organic layer was separated
10. dry with materialdried (MgSO4)
11. filtrationfiltered
12. customevaporated