반응 #63595

ord-9f193ad997424c4c8d6552e9e1529713

반응 방정식

[H][H]
hydrogen
c1ccsc1
thiophene
O=Cc1ccccc1
benzaldehyde
NC(=O)C1CNCCN1
2-piperazinecarboxamide
NC(=O)C1CN(Cc2ccccc2)CCN1
4-(phenylmethyl)-2-piperazinecarboxamide
수율 55.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the catalyst was filtered off
  2. 2
    기타the filtrate was evaporated
  3. 3
    여과The mixture was filtered
  4. 4
    기타to crystallize at room temperature
  5. 5
    여과The product was filtered off
  6. 6
    기타dried

실험 절차

To 1 part of a solution of 2 parts of thiophene in 40 parts of ethanol were added 2.2 parts of benzaldehyde, 2.6 parts of 2-piperazinecarboxamide and 120 parts of methanol. The whole was hydrogenated at normal pressure and at room temperature with 2 parts of platinum-on-charcoal catalyst 5%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The solid residue was boiled in 64 parts of acetonitrile. The mixture was filtered and the filtrate was allowed to crystallize at room temperature. The product was filtered off and dried, yielding 2.4 parts (55%) of 4-(phenylmethyl)-2-piperazinecarboxamide; mp. 168.3° C. (intermediate 36).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04766125uspto-grants-1988_08