反应详情

温度

-32 °C

A solution was prepared from 5.8 g of 1-benzyl-4,7- dihydro-1H-cyclopenta[1,2-c:3,4-c']dipyrazole in 150 ml of tetrahydrofuran and 300 ml of liquid ammonia at -78° C. Sodium metal (2.8 g) was added in small pieces and the reaction was stirred at -32° C. for 1.5 hours. Ammonium chloride (10 g) was added and the ammonia was allowed to evaporate over a period of 20 minutes. The residual reaction mixture was filtered and the filter cake was washed with ethanol. The combined filtrates were then concentrated under reduced pressure and the residue was triturated with ethyl acetate to give 4,7-dihydro-1H-cyclopenta[1,2-c:3,4-c']dipyrazole as a tan granular solid (50% yield) melting at about 180° C. with decomposition

1. customto evaporate over a period of 20 minutes
2. customThe residual reaction mixture
3. filtrationwas filtered
4. washthe filter cake was washed with ethanol
5. concentrationThe combined filtrates were then concentrated under reduced pressure
6. customthe residue was triturated with ethyl acetate