Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclohexene | HCID 8079 | — |
| Reactant | HCID 18183216 | HCID 18183216 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 18183148 | HCID 18183148 | — |
Reaction Steps
527 mg of 8-ethyl-9-methyl-5-(4-nitrophenyl)-11H-1,3-dioxolo[4,5-h)imidazo[1,2-c][2,3]benzodiazepine is mixed in 11 ml of ethanol with 5.4 ml of cyclohexene and 106 mg of palladium hydroxide on carbon (Pearlman's catalyst), and it is stirred for 3 hours at a bath temperature of 110° C. After catalyst is filtered out, it is concentrated by evaporation, and the residue is chromatographed on silica gel with ethyl acetate as an eluant. After combining the corresponding fractions and recrystallization from ethanol, 348 mg of 5-(4-aminophenyl)-8-ethyl-9-methyl-11H-1,3-dioxolo[4,5-h]imidazo[1,2-c][2,3]benzodiazepine with a melting point of 227-228° C. is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06323197B1 |
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| Source dataset | uspto-grants-2001_11 |
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| ORD ID | ord-a5be3787b35547b7b6c99c3e68123004 |
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| Source note | uspto-grants-2001_11 |
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