反应详情

Grams 2 2-[2-(4-methylpiperazin-1-yl)ethylthio] benzimidazole, 0.86 ml benzyl chloride, a 3.5 g aqueous solution containing 1.16 g NaOH and 7.5 ml N,N-dimethylformanide were refluxed for 6 hours, then the solid precipitate was filtered off, and the limpid solution was evaporated almost to dryness. The obtained residue was dissolved in chloroform and water and the extraction was carried out three times; the organic phase was washed, made anhydrous and then evaporated to dryness. The obtained residue was chromatographed on a column eluting with chloroform, methyl alcohol, cyclohexane, ammonium hydroxide (65:15:15:0.1). The fractions, which contained the compound, were evaporated to dryness and the residue which was taken up with boiling petroleum ether (80°-φ° C.) and separated from the insoluble oil, gave, on cooling 0.3 g 1-benzyl-2-[2-4- methylpiperazin-1-ethylthio]benzimidazole melting at 122°-125° C.

1. temperaturewere refluxed for 6 hours
2. filtrationthe solid precipitate was filtered off
3. customthe limpid solution was evaporated almost to dryness
4. dissolutionThe obtained residue was dissolved in chloroform
5. extractionwater and the extraction
6. washthe organic phase was washed
7. customevaporated to dryness
8. customThe obtained residue was chromatographed on a column
9. washeluting with chloroform, methyl alcohol, cyclohexane, ammonium hydroxide (65:15:15:0.1)
10. customwere evaporated to dryness
11. customwas taken up with boiling petroleum ether (80°-φ° C.)
12. customseparated from the insoluble oil
13. customgave