反应详情

Grams 2.2 2-mercapto-1H-benzimidazol and 2.4 g NaOH were dissolved in 40 ml 90% ethyl alcohol, then 3.5 g 1-(2-chloroethyl)-4-methylpiperazine hydrochloride were added thereto. The reaction mixture was refluxed for 2 hours, the solid precipitate removed by filtration, the limpid solution evaporated to dryness and the residue dissolved in chloroform and washed with water. The organic phase was made anhydrous, then evaporated to dryness and the residue chromatographed on a column eluting with chloroform, methyl alcohol, cyclohexane, ammonium hydroxide (68:15:15:0.2). The fractions which contained the product, were collected together and evaporated to dryness and the residue which was triturated with isopropyl ether, gave 0.65 g 2-[2-(4-methylpiperazin-1-yl)ethylthio] benzimidazole melting at 93°-95° C. (with a slight decomposition).

1. temperatureThe reaction mixture was refluxed for 2 hours
2. customthe solid precipitate removed by filtration
3. customthe limpid solution evaporated to dryness
4. dissolutionthe residue dissolved in chloroform
5. washwashed with water
6. customevaporated to dryness
7. customthe residue chromatographed on a column
8. washeluting with chloroform, methyl alcohol, cyclohexane, ammonium hydroxide (68:15:15:0.2)
9. customwere collected together
10. customevaporated to dryness
11. customthe residue which was triturated with isopropyl ether