Reaktion #63625

Reaktionsgleichung

ethyl 1-[4,4-bis(4-fluorophenyl)butyl]-4-[2-[(2,6-dichlorophenyl)amino]-2-oxoethyl]-2-piperazinecarboxylate

hydrochloric acid

sodium hydrogen carbonate

→

1-[4,4-bis(4-fluorophenyl)butyl]-4-[2-[(2,6-dichlorophenyl)amino]-2-oxoethyl]-2-piperazinecarboxylic acid

Lösungsmittel

2-Propanone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas obtained
2. 2
   Sonstigethe 2-propanone was evaporated
3. 3
   SonstigeThe aqueous phase was decanted
4. 4
   Temperaturwhile warming
5. 5
   FiltrationThe solid product was filtered off
6. 6
   TemperaturAfter cooling for a while
7. 7
   Filtrationthe less pure product was filtered off
8. 8
   Temperaturthe filtrate was cooled
9. 9
   FiltrationThe product was filtered off
10. 10
    Sonstigedried

Vorschrift

A mixture of 3.3 parts of ethyl 1-[4,4-bis(4-fluorophenyl)butyl]-4-[2-[(2,6-dichlorophenyl)amino]-2-oxoethyl]-2-piperazinecarboxylate and 60 parts of a hydrochloric acid solution 12N was stirred for 8 hours at 100° C. in an oil-bath. 2-Propanone was added whereupon a solution was obtained. The pH was adjusted to 5 with sodium hydrogen carbonate and the 2-propanone was evaporated: a sticky oil in water was remained. The aqueous phase was decanted and the sticky oil was taken up in 24 parts of 4-methyl-2-pentanone while warming. The solid product was filtered off and boiled in 120 parts of acetonitrile. After cooling for a while, the less pure product was filtered off and the filtrate was cooled. The product was filtered off and dried, yielding 0.31 parts of 1-[4,4-bis(4-fluorophenyl)butyl]-4-[2-[(2,6-dichlorophenyl)amino]-2-oxoethyl]-2-piperazinecarboxylic acid; mp. 204.3° C. (compound 172).

Quelle