反应详情

温度

140 °C

A mixture of 6-Chloro-3-phenyl-1,2,4-Triazolo[3,4-a] phthalazine (2.0 g, prepared according to procedures described in Zh. Org. Khim. (1975), 11(7), 1570–2 and J. Med. Chem. (1988), 31(6), 1115–23.) and copper cynaide (2.0 g) in 50 ml of DMSO is stirred at 140° C. overnight. The mixture is cooled, poured into water and extracted with methylene chloride. The organic layer is washed with water, dried over Na2SO4 and concentrated to give a tan solid which is then dissolved in 50 mL of methanol. The resulting solution is saturated with HCl gas and the mixture is stirred at room temperature overnight. 20 mL of water and 1 mL of 10 N NaOH solution are added, the resulting mixture is then heated under reflux for 4 hours. The methanol is then evaporated in vacuo, and the remaining mixture is diluted with water. After adjusting the pH to 4–5 with 1N HCl, the solid is collected by filtration, and dried to give the title compound as a solid.

1. temperatureThe mixture is cooled
2. extractionextracted with methylene chloride
3. washThe organic layer is washed with water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customto give a tan solid which
7. stirringthe mixture is stirred at room temperature overnight
8. temperaturethe resulting mixture is then heated
9. temperatureunder reflux for 4 hours
10. customThe methanol is then evaporated in vacuo
11. additionthe remaining mixture is diluted with water
12. filtrationthe solid is collected by filtration
13. customdried