反应详情

1-Chloro-6,7-dimethoxy phthalazine (2.25 g.), 3-hydroxymethylpiperidine (1.72 g.) and triethylamine (1.3 ml.) in iso-amyl alcohol (60 ml.) were heated at 95° C. for 42 hours. The cooled reaction mixture was then filtered and the filtrate was taken to dryness in vacuo. The residue was dissolved in water (100 ml.), 5 N sodium hydroxide solution was added to give a pH of 11 and the basic mixture was then extracted with chloroform (2×100 ml.). The chloroform extracts were combined, dried (MgSO4) and concentrated in vacuo to give a brown oil, which was triturated with ether (50 ml.) and filtered. The resultant solid was crystallized twice from acetonitrile, yielding 6,7-dimethoxy-1-(3-hydroxymethylpiperidino)phthalazine (1.83 g.), m.p. 162°-165° C.

1. customThe cooled reaction mixture
2. filtrationwas then filtered
3. dissolutionThe residue was dissolved in water (100 ml.)
4. addition5 N sodium hydroxide solution was added
5. customto give a pH of 11
6. extractionthe basic mixture was then extracted with chloroform (2×100 ml.)
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo
9. customto give a brown oil, which
10. customwas triturated with ether (50 ml.)
11. filtrationfiltered
12. customThe resultant solid was crystallized twice from acetonitrile