Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 21094301 | HCID 21094301 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 21094309 | HCID 21094309 | — |
Reaction Steps
The compound of Example 5 is dissolved in a minimum of methanol with the application of heat and then diluted with toluene. 1.5 equivalents of triethylamine are then added to the solution, and the reaction mixture is subsequently heated at reflux in the presence of palladium-on-carbon (10% by weight) for 3 hours. After removal of the catalyst by filtration, the solution is evaporated under reduced pressure. The oil obtained is purified by chromatography on silica gel (eluant dichlormethane/methanol 9/1). The purified oil is taken up in ether saturated with HCl(g) and stirred until a precipitate is obtained. The precipitate so formed is suction-filtered off and placed under vacuum in a dessicator. The title product is obtained in the form of a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07214689B2 |
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| Source dataset | uspto-grants-2007_05 |
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| ORD ID | ord-70c087362542495dad0b48d0c75786dc |
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| Source note | uspto-grants-2007_05 |
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