Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-(Bromomethyl)pyridine hydrobromide | HCID 2734720 | — |
| Reactant | (3S,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-3-methylpiperidin-2-one | HCID 58574008 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58573766 | HCID 58573766 | — |
Reaction Steps
To a solution of (3S,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-3-methylpiperidin-2-one (2.246 g, 6 mmol; Example 71D) in DMF (25 mL) was added sodium hydride, 60% dispersion in mineral oil (0.504 g, 12.60 mmol) and the mixture was stirred at 0° C. for 5 minutes. To this was added 2-(bromomethyl)pyridine hydrobromide (1.593 g, 6.30 mmol) at 0° C. The resulting mixture was stirred at 0° C. for 10 min and quenched with saturated NH4Cl solution, extracted with EtOAc, washed with sat. aq. NaCl solution, dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by flash chromatography on silica gel (eluent: 0 to 100% EtOAc in hexanes) to give the title compound. Mass Spectrum (ESI) m/z=465 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09296736B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-fedfce11c9c349da94682cabd1c6b632 |
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| Source note | uspto-grants-2016_03 |
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