反应详情

温度

50 °C

A stainless steel bomb was charged with 2,3-dimethoxy-5-nitropyridine (430 mg, 2335 μmol), 10% Pd/C (124 mg, 1168 μmol) and 4.7 mL EtOAc. The vessel was sealed and was purged with hydrogen once, before filling with hydrogen at a pressure of 2 attn. The reaction mixture was heated at 50° C. for 3 h. Upon cooling, the mixture was filtered through a pad of Celite, rinsing with EtOAc. The filtrate was concentrated and passed through a silica plug using 5% MeOH/DCM. The filtrate was concentrated to provide 5,6-dimethoxypyridin-3-amine as a peach colored oil that crystallized upon standing. GC/MS confirmed the correct mass to be [M+H]=155.

1. customThe vessel was sealed
2. customwas purged with hydrogen once
3. temperatureUpon cooling
4. filtrationthe mixture was filtered through a pad of Celite
5. washrinsing with EtOAc
6. concentrationThe filtrate was concentrated
7. concentrationThe filtrate was concentrated