反应详情

A mixture of 2-(2-chloroethyl)-6,7-dimethoxy-1(2H)-phthalazinone (2.68 g; 0.01 mole) obtained as described in Example 2, N-phenyl piperazin (1.5 ml), triethyl amine (2.78 ml) and potassium iodide (0.16 g; 0,001 mole) in acetonitrile (50 ml), is refluxed for 12 hours. The solvent is evaporated under reduced pressure and the residue is dissolved in dilute HCl, washed with methylene chloride and after alkalinization with NaHCO3, the mixture is extracted with methylene chloride, dried on sodium sulphate, filtered and evaporated. The residue is dissolved in acetone, made acid with HCl in ethyl ether and the product which separates is filtered and recrystallized from 95% ethanol to give 2-[2-(4-phenylpiperazin-1-yl)-ethyl]-6,7-dimethoxy-1(2H)-phthalazinone dihydrochloride (m.p. 222°-226° C.).

1. customobtained
2. temperatureis refluxed for 12 hours
3. customThe solvent is evaporated under reduced pressure
4. dissolutionthe residue is dissolved in dilute HCl
5. washwashed with methylene chloride
6. extractionafter alkalinization with NaHCO3, the mixture is extracted with methylene chloride
7. customdried on sodium sulphate
8. filtrationfiltered
9. customevaporated
10. dissolutionThe residue is dissolved in acetone
11. filtrationthe product which separates is filtered
12. customrecrystallized from 95% ethanol