反应详情

A mixture of 1.14 gm of 2-piperazino 5-chloro pyridine, 1.35 gm of 1-(3-chloro propyl)-2,3-dihydro-1H-benzimidazol-2-one (available from Janssen) and 1.49 gm of diisopropylethylamine in 3 ml DMF and 30 ml toluene is kept for 12 hours at 110° C. Upon cooling to ambient temperature, 30 ml water is added and the mixture is extracted with chloroform (CHCl3) and the extract is collected, washed with 20 ml water and dried over sodium sulfate (Na2SO4). The crude product (2.5 gm) which is obtained after removing the solvents is purified using chromatography: solid phase (SiO2 ; 40 μm; Baker); eluant 2% methanol (CH3OH) in methylene chloride (CH2Cl2). A sample of this purified material (1.2 gm) was transferred into its hydrochloride (mp: 200° C.) by treating an ethanolic suspension of this material with a mixture of ethyl ether/HCl.

1. extractionthe mixture is extracted with chloroform (CHCl3)
2. customthe extract is collected
3. washwashed with 20 ml water
4. dry with materialdried over sodium sulfate (Na2SO4)