Sodium Carbonate → 4-[4,4-bis(4-fluorophenyl)butyl]-2-[(methylamino)carbonyl]-N-(2,4,6-trimethylphenyl)-1-piperazineacetamide

Participants

Reaction Steps

A mixture of 5.8 g of 4-[4,4-bis(4-fluorophenyl)butyl]-N-methyl-2-piperazine-carboxamide, 3.6 g of 2-chloro-N-(2,4,6-trimethylphenyl)acetamide, 2.12 g of sodium carbonate and 150 ml of MIK is stirred and refluxed for 18 hours. The reaction mixture is cooled and washed with water. The organic phase is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is dried, yielding 4.34 g of 4-[4,4-bis(4-fluorophenyl)butyl]-2-[(methylamino)carbonyl]-N-(2,4,6-trimethylphenyl)-1-piperazineacetamide (compound 2, mp. 90.2° C.).

Provenance & Evidence