反应详情

温度

2 °C

2-Bromoacetyl-4-methoxypyridine (11.5 g, 0.05) and 2-chlorobenzimidazole (7.5 g, 0.05 mole) were dissolved in dimethylformamide (75 ml) and cooled to 2° C. K2CO3 (12 g, 0.08 mole) was added and the temperature rose to 9° C. as the suspension was stirred for 1/2 hour. The mixture was added to H2O (200 ml) giving a solid which was removed by filtration. The mother liquors were extracted with ethyl acetate and the solid was dissolved in the extracts. The organic solution was washed (brine) and dried (MgSO4) and purified by passage down a silica column and evaporated to dryness to give a sticky solid. Trituration with propan-2-ol/di-isopropyl ether gave 2-chloro-1-[2-(2-[4-methoxypyridyl])-2-oxoethyl]-benzimidazole (7.2 g).

1. customrose to 9° C. as the suspension
2. customgiving a solid which
3. customwas removed by filtration
4. extractionThe mother liquors were extracted with ethyl acetate
5. dissolutionthe solid was dissolved in the extracts
6. washThe organic solution was washed (brine)
7. dry with materialdried (MgSO4)
8. custompurified by passage down a silica column
9. customevaporated to dryness
10. customto give a sticky solid