Potassium Iodide → HCID 67925653, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 5.5 parts of cis-N-(3-methoxy-4-piperidinyl-N-methyl-2-benzothiazolamine ethanedioate(1:1), 10.6 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone was stirred and refluxed for 30 minutes. After cooling to 60° C., 4.4 parts of 1-chloro-4-(4-chlorobutoxy)benzene were added. The whole was stirred and refluxed overnight. After cooling, water was added and the layers were separated. The organic layer was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the ethanedioate salt in 2-propanol. The salt was filtered off and dried, yielding 6 parts (73%) of cis-N-[1-[4-(4-chlorophenoxy)butyl]-3-methoxy-4-piperidinyl]-N-methyl-2-benzothiazolamine ethanedioate(1:1); mp. 210.4° C. (205).

Provenance & Evidence