Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | HCID 66717842 | HCID 66717842 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67361367 | HCID 67361367 | — |
Reaction Steps
To a stirred mixture of 3-bromo-8-chloro-6-hydroxyquinoline (5.0 g) (preparation described in WO 2004/108663), sodium iodide (5.8 g) and copper iodide (0.37 g) in dioxane (65 ml) is added N,N″-dimethyl-ethane-1,2-diamine (0.34 g) in a sealed tube under argon. The mixture is stirred at 120° C. for 14 h and upon cooling is treated with aqueous ammonia followed by aqueous hydrochloric (to pH 5). Extraction with ethyl acetate, drying of the organic phase over magnesium sulphate, filtration and evaporation under reduced pressure gives the required product ((M+1)+306) that is used as such in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08440595B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-7af200d2b98a444eacbdbc0a0b5088ff |
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| Source note | uspto-grants-2013_05 |
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