反応 #1476500

ord-1a4e50530b374f4c9abb7ac5ab51f325

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度refluxed for 2 hours
  2. 2
    温度The reaction mixture is cooled
  3. 3
    洗浄washed with a diluted ammonium hydroxide solution
  4. 4
    その他the layers are separated
  5. 5
    その他The organic phase is dried
  6. 6
    ろ過filtered
  7. 7
    その他evaporated
  8. 8
    その他The residue is crystallized from a mixture of methylbenzene and 2,2'-oxybispropane (20:20 by volume)
  9. 9
    ろ過The product is filtered off
  10. 10
    その他dried

実験手順

A mixture of 1.9 parts of 5-[4-(diphenylmethyl)-1-piperazinylmethyl]-1-methyl-1H-benzimidazole-2-methanol, 1.55 parts of acetic acid anhydride and 45 parts of methylbenzene is stirred and refluxed for 2 hours. The reaction mixture is cooled, washed with a diluted ammonium hydroxide solution and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is crystallized from a mixture of methylbenzene and 2,2'-oxybispropane (20:20 by volume). The product is filtered off and dried, yielding 1.5 parts (74.4%) of {5-[4-(diphenylmethyl)-1-piperazinylmethyl]-1-methyl-1H-benzimidazol-2-ylmethyl}acetate; mp. 201.1° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04243806uspto-grants-1981_01