反应详情

温度

60 °C

5-Methyl-3-phenylindazole (400 g) was dissolved in toluene (1 l) and 1,3-dibromopropane (600 ml), and to the solution were added triethylbenzylammonium chloride (40 g) and 30% aqueous sodium hydroxide (800 ml). The mixture was heated at 60° C. for 30 minutes while stirring and the resulting organic layer was separated. The layer was washed with water, dried over sodium sulfate and then heated at reflux for 3 hours. The precipitate was recovered by filtration and washed with toluene to give 319 g of 2,3-dihydro-7-methyl-9-phenyl-1H-pyrazolo[1,2-a]indazolium bromide. The product which was recrystallized from water had a decomposition point of 239° C.

1. customthe resulting organic layer was separated
2. washThe layer was washed with water
3. dry with materialdried over sodium sulfate
4. temperatureheated
5. temperatureat reflux for 3 hours
6. filtrationThe precipitate was recovered by filtration
7. washwashed with toluene