Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Aminopyridine | HCID 10439 | — |
| Reactant | p-Bromophenethylamine | HCID 533915 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 64135446 | HCID 64135446 | 24.8% |
Reaction Steps
In a sealed tube, a mixture of 1.9 g (20.4 mmol) of 2-aminopyridine and 6.1 g (30.6 mmol) of 4-bromophenethylamine dissolved in butanol (10 ml) is heated at 230° C. for 1 hour by microwave. The mixture, cooled to room temperature, is poured into water (50 ml) and extracted with ethyl acetate (3×100 ml), and the combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue is purified by flash chromatography on a column of silica gel (eluent: dichloromethane/ethyl acetate, from 0% to 50% ethyl acetate). 1.4 g of product are obtained in the form of a white powder. Yield: 24%. Melting point: 71° C. MH+: 278.1 (tr: 3.71 min., condition 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08436011B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-81b7b9c127374021bda5c1fbd5e92d92 |
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| Source note | uspto-grants-2013_05 |
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