Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl morpholine oxide | HCID 82029 | — |
| Reactant | HCID 58573815 | HCID 58573815 | — |
| Reactant | Jones' reagent | HCID 131709961 | — |
| Catalyst | Osmium Tetroxide | HCID 30318 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 56591284 | HCID 56591284 | — |
Reaction Steps
To a solution of (3S,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-3-methyl-1-(4-methylpyridin-2-yl)piperidin-2-one (Example 114, Step A) (73 mg, 0.16 mmol) in 780 μL of tetrahydrofuran was added water (1.0 mL), followed by 2-methylpropan-2-ol (100 μL) at room temperature. The reaction mixture was treated with 4-methylmorpholine 4-oxide (28 mg, 0.24 mmol), followed by osmium tetroxide (2.0 mg, 7.8 μmol) and was stirred at room temperature for 2 hours. The reaction mixture was treated with a 1.25 M solution of Jones reagent (190 μL, 0.24 mmol) at room temperature and was stirred at room temperature for 1 hour. The reaction was quenched with water and extracted (3×EtOAc). The combined organic layers were washed with sat. aq. NaCl solution, dried over Na2SO4, filtered and the filtrate was concentrated under reduced pressure. Purification of the residue by HPLC on an Eclipse column (Agilent Technologies, Santa, Clara, Calif.) (20 to 80% acetonitrile/water, gradient elution) provided the title compound as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08569341B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-6bb07ac4130b412fbf764f12c5d19e65 |
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| Source note | uspto-grants-2013_10 |
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