Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 178520208 | HCID 178520208 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Product | HCID 178478666 | HCID 178478666 | 93% |
Reaction Steps
Ethanol (200 mL) was added to a mixture of 2-(4-nitroimidazolyl)-2-phenyl-1-pyrrolidinylethan-1-one (3) (0.752 g, 2.8 mm) and 10% Pd on carbon (75 mg) in a Bradley hydrogenation apparatus. The stirred reaction mixture was subjected to a 60 psi H2 atmosphere and warmed to 60° C. After 2 hours, the reaction mixture was cooled to room temperature and the catalyst was removed by filtration. Anhydrous HCl gas was added to the filtered solution until saturation. The volatiles were then removed under vacuum to give a light yellow foam. Diethyl ether and methylene chloride (25:1) were added to the foam and the resulting mixture was stirred overnight to achieve crystallization. The resulting slurry was filtered and the cake was washed with diethyl ether. The cake was dried under vacuum to give 0.659 g (93%) of a yellow solid. LGD 208.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06639076B1 |
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| Source dataset | uspto-grants-2003_10 |
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| ORD ID | ord-6e0060a37aa64ef4ac350f6fe753b036 |
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| Source note | uspto-grants-2003_10 |
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