反应详情

2-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-8,10,10-trimethyl-10H-pyrido[1,2-a]indolylium perchlorate (36 g, 0.077 mol; Sigma-Aldrich) was added to a conical 1-L flask equipped with magnetic stir bar, followed by 480 mL of CH2Cl2—CH3OH mixture (3:2). Stirring was started and hydrazine monohydrate (25 g, 0.50 mol; Aldrich) was added to the reaction mixture at once. Stirring was continued until all solid was dissolved. The flask was closed with a stopper and let to stand at room temperature overnight without stirring. After about 16 hours the precipitated solid phthalhydrazide was filtered off, washed with 100 mL of CH2Cl2—CH3OH mixture (3:2) and discarded. The combined filtrates were evaporated and the resulted solid was washed with Ether-CH3OH. The solid was filtered, washed with ether and dried. The yield was 26 g (100% of theory).

1. customequipped with magnetic stir bar
2. stirringStirring
3. dissolutionwas dissolved
4. customThe flask was closed with a stopper
5. stirringwithout stirring
6. filtrationAfter about 16 hours the precipitated solid phthalhydrazide was filtered off
7. washwashed with 100 mL of CH2Cl2—CH3OH mixture (3:2)
8. customThe combined filtrates were evaporated
9. washthe resulted solid was washed with Ether-CH3OH
10. filtrationThe solid was filtered
11. washwashed with ether
12. customdried