Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium periodate | HCID 23667635 | — |
| Reactant | HCID 90218975 | HCID 90218975 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 90219100 | HCID 90219100 | 49.2% |
Reaction Steps
To a solution of (racemic)-tert-butyl N-[[(1S,2S,4S)-2-[(tert-butoxycarbonylamino)methyl]-4-(2-hydroxyethyl)cyclohexyl]methyl]carbamate (772 mg, 2 mmol) in acetonitrile (3 mL), carbon tetrachloride (3 mL) and water (4.5 mL) is added sodium periodate (1.28 g, 6 mmol) followed by RuCl3.H2O (21 mg, 0.1 mmol). The resulting mixture is stirred for 2 hr then diluted with EtOAc, washed with brine, dried over MgSO4 and concentrated. The residue is taken up in saturated sodium carbonate solution and extracted with EtOAc. The aqueous phase is acidified with HCl (2M aqueous) and extracted with EtOAc. The organic extract is washed with brine, dried over MgSO4 and concentrated. This residue is purified by silica chromatography (eluting with ethyl acetate) to give the title compound (394 mg) as a viscous oil. 1H NMR (DMSO-d6) δ 0.7-1.0 (m, 1H), 1.0-1.9 (m, 9H), 1.39 (s, 18H), 2.0-2.3 (m, 2H), 2.6-3.18 (m, 4H), 6.6-6.8 (bm, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08912169B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-96b1929df4ce498d975582ab23457ff2 |
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| Source note | uspto-grants-2014_12 |
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