Triethylamine → Mioflazine Hydrochloride

Participants

Reaction Conditions

Reaction Steps

A mixture of 4.05 parts of 2-chloro-N-(2,6-dichlorophenyl)acetamide, 5.6 parts of 1-[4,4-bis(4-fluorophenyl)butyl]-2-piperazinecarboxamide, 2.94 parts of N,N-diethylethanamine and 63 parts of N,N-dimethylformamide was stirred for 5 hours at 70° C. The reaction mixture was poured onto ice-water. The precipitated product was filtered off and dissolved in dichloromethane. The solution was washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the hydrochloride salt in 2-propanone and 2-propanol. The salt was filtered off and stirred for 30 minutes in 1,1'-oxybisethane, yielding 4.54 parts of 3-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dichlorophenyl)-1-piperazineacetamide dihydrochloride monohydrate; mp. 182.7° C. (compound 72).

Provenance & Evidence