反应详情

A solution of 7-methoxy-2-(4-phthalimidobutyl)-1,2,3,4-tetrahydroisoquinoline (17.4 g 0.0478 mol) and hydrazine monohydrate (4.6 ml, 0.095 mol) in ethanol (300 ml) were stirred at room temperature for 18 h and at reflux for 1 h. The cooled reaction mixture was filtered and the filtrate evaporated in vacuo. The residue was dissolved in 2.5N hydrochloric acid, filtered through Kieselguhr and the filtrate basified with 0.880 ammonia. The product was extracted into dichloromethane (4×200 ml), the combined extracts were dried (Na2SO4) and evaporated in vacuo to afford the title compound as a brown oil (7 g, 63%).

1. temperatureat reflux for 1 h
2. customThe cooled reaction mixture
3. filtrationwas filtered
4. customthe filtrate evaporated in vacuo
5. dissolutionThe residue was dissolved in 2.5N hydrochloric acid
6. filtrationfiltered through Kieselguhr
7. extractionThe product was extracted into dichloromethane (4×200 ml)
8. dry with materialthe combined extracts were dried (Na2SO4)
9. customevaporated in vacuo