반응 #4405

반응 방정식

K2CO3

2-Bromoacetyl-4-methoxypyridine

2-chlorobenzimidazole

H2O

→

propan-2-ol di-isopropyl ether

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타rose to 9° C. as the suspension
2. 2
   기타giving a solid which
3. 3
   기타was removed by filtration
4. 4
   추출The mother liquors were extracted with ethyl acetate
5. 5
   workup.DISSOLUTIONthe solid was dissolved in the extracts
6. 6
   세척The organic solution was washed (brine)
7. 7
   건조dried (MgSO4)
8. 8
   기타purified by passage down a silica column
9. 9
   기타evaporated to dryness
10. 10
    기타to give a sticky solid

실험 절차

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).

출처