反応 #1476492

反応方程式

5-[4-(diphenylmethyl)-1-piperazinylmethyl]-1-ethyl-1H-benzimidazole

sodium amide

N,N-dimethylbenzenamine

→

5-[4-(diphenylmethyl)-1-piperazinylmethyl]-1-ethyl-1H-benzimidazol-2-amine

反応条件

後処理

1. 1
   workup.STIRRINGStirring at 135° C.
2. 2
   温度The reaction mixture is cooled
3. 3
   workup.ADDITIONpoured onto water
4. 4
   抽出The product is extracted with trichloromethane
5. 5
   その他The extract is dried
6. 6
   ろ過filtered
7. 7
   その他evaporated
8. 8
   その他The residue is purified by column-chromatography over silica gel using
9. 9
   workup.ADDITIONa mixture of trichloromethane and methanol (95:5 by volume)
10. 10
    その他The pure fractions are collected
11. 11
    その他the eluent is evaporated
12. 12
    その他The residue is crystallized from methylbenzene
13. 13
    ろ過The product is filtered off
14. 14
    その他dried

実験手順

A mixture of 4.1 parts of 5-[4-(diphenylmethyl)-1-piperazinylmethyl]-1-ethyl-1H-benzimidazole, 1.2 parts of sodium amide and 20 parts of N,N-dimethylbenzenamine is stirred and heated slowly to 135° C. Stirring at 135° C. is continued for 3 hours. The reaction mixture is cooled and poured onto water. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) and a small amount of ammonium hydroxide as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from methylbenzene. The product is filtered off and dried, yielding 1.5 parts of 5-[4-(diphenylmethyl)-1-piperazinylmethyl]-1-ethyl-1H-benzimidazol-2-amine; mp. 214.3° C.

出典