Oxalic Acid → HCID 131719594, compound

Participants

Reaction Steps

The procedure is carried out as in Example 11, using 1.15 g of 3-(3-chloropropyl)-1,1-dimethyl-5-fluoro-4-oxo-1,2,3,4-tetrahydro-3,1-benzazasiline, 1.1 cm3 of triethylamine and 1.3 g of 1-phenylpiperazine in 23 cm3 of toluene (23 cc). After purification by flash chromatography on a silica column under a nitrogen stream at moderate pressure (0.5-1.5 bar) with a dichloromethane-methanol mixture (98.5-1.5 by volume) as eluent, 0.3 g of 1,1-dimethyl-5-(4-phenyl-1-piperazinyl)-3- [3-(4-phenyl-1-piperazinyl)-propyl]-4-oxo-1,2,3,4-tetrahydro-3,1-benzazasiline; melting point =166° C., and 0.3 g of an oil are obtained, which oil, when dissolved in 3 cm3 of acetone and treated with 0.24 g of oxalic acid, yield 1,1-dimethyl-5-fluoro-4-oxo-3-3-(4-phenyl-1-piperazinyl) 3-propyl]-1,2,3,4,-tetrahydro-3,1-benzazasiline in the oxalate form; melting point =99° C.

Provenance & Evidence