HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 11394118, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 67241489 | HCID 67241489 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11394118 | HCID 11394118 | 78% |
Reaction Steps
10.89 g (28 mmoles) 8-chloro-4-methyl-1-(3-methyl-4-nitrophenyl)-3H-2,3-benzodiazepine 3-carboxylic acid methyl amide are dissolved in the mixture of 190 ml of methanol and 95 ml of dichloromethane, and about 5.0 g of wet Raney nickel catalyst and 3.5 ml (70 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 dichloro-methane, the filtrate is evaporated and the residue is solidified by rubbing with 100 ml of water. The crude product is recrystallized from ethanol. Thus 7.73 g (78%) of the desired compound melting at 210-212° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960375B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-f389e4b753be4c20bac71c0b2398838a |
| Source note | uspto-grants-2011_06 |