Реакция #442182

Уравнение реакции

1-(3-chloropropyl)-1H-benzimidazole

4-(diphenylmethoxy)piperidine hydrochloride

sodium carbonate

4-methyl-2-pentanone

→

1-{3-[4-(diphenylmethoxy)-1-piperidinyl]propyl}-1H-benzimidazole

Растворители

water

water

Условия реакции

Обработка

1. 1
   ТемператураThe reaction mixture is cooled
2. 2
   Другоеthe layers are separated
3. 3
   СушкаThe 4-methyl-2-pentanone-phase is dried
4. 4
   Фильтрацияfiltered
5. 5
   Другоеevaporated
6. 6
   ДругоеThe oily residue is purified by column-chromatography over silica gel using
7. 7
   workup.ADDITIONa mixture of trichloromethane and methanol (95:5 by volume) as eluent
8. 8
   ДругоеThe pure fractions are collected
9. 9
   Другоеthe eluent is evaporated
10. 10
    ДругоеThe oily residue is crystallized from 2,2'-oxybispropane
11. 11
    ФильтрацияThe product is filtered off
12. 12
    Другоеdried

Методика

A mixture of 6 parts of 1-(3-chloropropyl)-1H-benzimidazole, 7.6 parts of 4-(diphenylmethoxy)piperidine hydrochloride, 10.6 parts of sodium carbonate and 200 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled, water is added and the layers are separated. The 4-methyl-2-pentanone-phase is dried, filtered and evaporated. The oily residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The oily residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 1-{3-[4-(diphenylmethoxy)-1-piperidinyl]propyl}-1H-benzimidazole; mp. 110.2° C.

Источник