反应详情

A solution of 5.0 g of 6-chloro-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine and 10.0 g of 1-(2-aminoethyl)pyrrolidine in 50 ml of 2-methoxyethanol was heated at reflux for 15 hours. The solution was then concentrated and the resulting residue was partitioned between methylene chloride and saturated aqueous sodium bicarbonate solution. The organic layer was separated, dried over sodium sulfate and concentrated. The concentrate was triturated with ether and the solid which formed was separated by filtration to give 6-[2-(1-pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine melting at about 160°-162° C. after recrystallization from a mixture of toluene and hexane. This compound has the following structural formula ##STR3##

1. temperatureat reflux for 15 hours
2. concentrationThe solution was then concentrated
3. customthe resulting residue was partitioned between methylene chloride and saturated aqueous sodium bicarbonate solution
4. customThe organic layer was separated
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe concentrate was triturated with ether
8. customthe solid which formed
9. customwas separated by filtration