Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 19699106 | HCID 19699106 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19699095 | HCID 19699095 | 76.8% |
Reaction Steps
A mixture of 2.0 g of 6-(4-nitrobenzoyl)-1,4,5,6-tetrahydropyrazolo[3,4-d]thieno[3,2-b]azepine in 40 ml of absolute ethanol is stirred under argon while 1.6 ml of hydrazine is added. The reaction mixture is heated at 60° C. for 1.5 hours. The reaction mixture is cooled to room temperature and 400 mg of 10% Pd/C added and the reaction mixture heated at 100° C. for 1.5 hours. The reaction mixture is filtered through diatomaceous earth and the cake washed with methylene chloride. The filtrate is concentrated in vacuo to a residue which is crystallized from ethyl acetate:hexane to give 1.4 g of the desired product as yellow crystals, 242°-260° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05719278 |
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| Source dataset | uspto-grants-1998_02 |
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| ORD ID | ord-57951aa35c194b3e9c080edd6d143dd6 |
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| Source note | uspto-grants-1998_02 |
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