Reaktion #63576

Reaktionsgleichung

2-chloroacetyl chloride

4-fluoro-α-(4-fluorophenyl)benzenemethanamine

sodium carbonate

→

N-[bis(4-fluorophenyl)-methyl]-2-chloroacetamide

Lösungsmittel

2-propanone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat a temperature below 30° C. (cooling in an ice-bath was necessary)
2. 2
   Temperaturat reflux
3. 3
   Filtrationthe sodium carbonate was filtered off
4. 4
   Waschenwashed with 2-propanone
5. 5
   SonstigeThe filtrate was evaporated
6. 6
   Sonstigethe residue was crystallized from 2,2'-oxybispropane

Vorschrift

To a stirred solution of 21.9 parts of 4-fluoro-α-(4-fluorophenyl)benzenemethanamine in 160 parts of 2-propanone were added 11.66 parts of sodium carbonate. Then there were added dropwise 12.43 parts of 2-chloroacetyl chloride at a temperature below 30° C. (cooling in an ice-bath was necessary). Upon completion, stirring was continued first for one hour at room temperature and further for 2 hours at reflux. After cooling to room temperature, the sodium carbonate was filtered off and washed with 2-propanone. The filtrate was evaporated and the residue was crystallized from 2,2'-oxybispropane, yielding 20.6 parts of N-[bis(4-fluorophenyl)-methyl]-2-chloroacetamide; mp. 127.6° C. (intermediate 4).

Quelle