HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 178462998, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 22758787 | HCID 22758787 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178462998 | HCID 178462998 | 97% |
Reaction Steps
A mixture of 11.0 g. of 4-chloro-1-ethyl-10,11-dihydrobenzo[4,5]cyclohepta[1,2-b]pyrazolo[4,3-e]pyridin5(1H)one (0.035 mol.), 4.5 g. of hydrazine hydrate 98% (0.09 mol.) and 125 ml. of abs. ethanol is refluxed for 3 hours with stirring. Then the reaction solution is filtered while hot and allowed to crystallize in a refrigerator. The crystallized 2,5,7,8-tetrahydro-5-ethyl-1,2,4,5,6-pentaazabenzo[6,7]cyclohepta[1,2,3-cd]-as-indacene which is filtered off, washed with alcohol and ether, melts at 229°-231°. Evaporation of the mother liquor to dryness and treatment with water yields a further crop of 1.9 g. of the product. Total yield 97%. Recrystallization from ethanol elevates the melting point to 230°-232°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04013672 |
| Source dataset | uspto-grants-1977_03 |
| ORD ID | ord-75eb154db5764226a72539b031914b8e |
| Source note | uspto-grants-1977_03 |