Reaktion #63595

Reaktionsgleichung

hydrogen

thiophene

benzaldehyde

2-piperazinecarboxamide

→

4-(phenylmethyl)-2-piperazinecarboxamide

Ausbeute 55.0%

Lösungsmittel

methanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthe catalyst was filtered off
2. 2
   Sonstigethe filtrate was evaporated
3. 3
   FiltrationThe mixture was filtered
4. 4
   Sonstigeto crystallize at room temperature
5. 5
   FiltrationThe product was filtered off
6. 6
   Sonstigedried

Vorschrift

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).

Quelle