Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Calcium Chloride | HCID 5284359 | — |
| Reactant | HCID 69209154 | HCID 69209154 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69214348 | HCID 69214348 | 1.1% |
Reaction Steps
6,7-Dichloro-2-{4-[2-(4-morpholinyl)ethoxy]-3-nitrophenyl}-1H-imidazo[4,5-b]pyridine (Example 246) (200 mg), zinc powder (200 mg) and anhydrous CaCl2 (500 mg) were mixed in 95% EtOH (20 ml) and heated (70° C., 4 h). The reaction mixture was allowed to cool and then filtered and evaporated in vacuo. The residue was dissolved in acetonitrile and subjected to semi-preparative HPLC-C18. The appropriate fraction was evaporated in vacuo and the residue dissolved in EtOAc (5 ml). This solution was washed with saturated aqueous NaHCO3 (5 ml) and brine (2 ml). The organic phase was dried (MgSO4) and evaporated in vacuo to afford the pure product (2 mg, 1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07410966B2 |
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| Source dataset | uspto-grants-2008_08 |
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| ORD ID | ord-6faad0cbd51044038b037df089711cdc |
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| Source note | uspto-grants-2008_08 |
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