تفاعل #4405

معادلة التفاعل

K2CO3

2-Bromoacetyl-4-methoxypyridine

2-chlorobenzimidazole

H2O

→

propan-2-ol di-isopropyl ether

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىrose to 9° C. as the suspension
2. 2
   أخرىgiving a solid which
3. 3
   أخرىwas removed by filtration
4. 4
   استخلاصThe mother liquors were extracted with ethyl acetate
5. 5
   workup.DISSOLUTIONthe solid was dissolved in the extracts
6. 6
   غسيلThe organic solution was washed (brine)
7. 7
   تجفيفdried (MgSO4)
8. 8
   أخرىpurified by passage down a silica column
9. 9
   أخرىevaporated to dryness
10. 10
    أخرىto give a sticky solid

الإجراء التجريبي

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).

المصدر