Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tributylstannane | HCID 5948 | — |
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | HCID 67461671 | HCID 67461671 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 67463862 | HCID 67463862 | — |
Reaction Steps
A solution of tributyltin hydride (3.88 mL) and 2,2′-azobis(isobutyronitrile) (0.56 g) in benzene (25 mL) was added dropwise to a solution of 1-(3-bromopropionyl)-2-(4-fluorophenyl)-2,3-dihydro-1H-pyridin-4-one obtained above (2.9 g) in benzene (60 mL) at 90° C. over four hours. The reaction solution was stirred at the same temperature for three hours. The reaction solution was returned to room temperature and poured into water, followed by extraction with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (heptane-ethyl acetate system) to obtain 600 mg of the title compound. The property values of the compound are as follows.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08048878B2 |
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| Source dataset | uspto-grants-2011_11 |
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| ORD ID | ord-0345054455074382a2205133449c508f |
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| Source note | uspto-grants-2011_11 |
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