Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 57099057 | HCID 57099057 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 14126714 | HCID 14126714 | 50% |
Reaction Steps
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
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04734430 |
|---|
| Source dataset | uspto-grants-1988_03 |
|---|
| ORD ID | ord-597c878c378d4f648ec7490badd5c999 |
|---|
| Source note | uspto-grants-1988_03 |
|---|