反应详情

温度

160 °C

A mixture of 7-chloro-4-methoxy-6-azaindole (1.029 g, 5.62 mmol), 1,2,4-triazole (11.6 g, 30 equiv), copper bronze (0.72 g, 11.2 mgatom) and finely pulverized KOH (0.63 g, 11.2 mmol) was heated in a sealed tube at 160° C. (oil bath temperature) for 18 h. The cooled mixture was taken up in MeOH and the resulting slurry was filtered through a pad of Celite. The filtrate was evaporated, the residue taken up in EtOAc and the resulting suspension was filtered. This process was repeated and the resulting solution was susequently adsorbed on silica gel and the volatiles were removed in vacuo. This solid was applied to the top of a silica gel chromatography column, which was eluted with 10-50% EtOAc—CH2Cl2 to give the title compound (0.697 g, 58%) as an off-white solid:

1. filtrationthe resulting slurry was filtered through a pad of Celite
2. customThe filtrate was evaporated
3. filtrationthe resulting suspension was filtered
4. customthe volatiles were removed in vacuo
5. washwas eluted with 10-50% EtOAc—CH2Cl2