HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 11245990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 67243228 | HCID 67243228 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11245990 | HCID 11245990 | 90.1% |
Reaction Steps
1.38 g (3.35 mmoles) of 8-chloro-4-methyl-1-(3-methyl-4-nitrophenyl)-3H-2,3-benzodiazepine-3-carboxylic acid cyclopropyl amide is dissolved in the mixture of 28 ml of methanol and 14 ml of dichloromethane, and about 1.0 g of wet Raney nickel catalyst and 0.42 ml (8.37 mmoles) of 98% hydrazine hydrate are subsequently added to it under vigorous stirring. The mixture is stirred for further 1 hour, the catalyst is filtered off, washed with dichloromethane, the filtrate is evaporated and the residue is solidified by rubbing with 10 ml of water. The crude product is recrystallized from ethanol. Thus 1.15 g (90%) of the desired compound melting at 233-236° C. is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960375B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-bf06418013404415a496beb2b0745655 |
| Source note | uspto-grants-2011_06 |