Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 57445556 | HCID 57445556 | — |
| Product | HCID 59808798 | HCID 59808798 | 89.9% |
Reaction Steps
A mixture of tert-butyl 4-[3-fluoro-5-(methylsulfonyl)phenyl]-4-hydroxypiperidine-1-carboxylate (3.3 g, 8.8 mmol) and polyphosphoric acid (20 ml) was heated at 120° C. for 3 h. The mixture was poured on to ice and was basified with 5 M sodium hydroxide. The mixture was extracted with ethylacetate (3×100 ml) and the combined organic phases was dried (MgSO4), evaporated and purified by flash column chromatography (methanol/ethylacetate 1:1) to give the title compound (2.02 g). MS m/z (rel. intensity, 70 eV) 255 (M+, bp), 254 (50), 251 (87), 172 (87), 146 (53).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08501777B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-821080415fa3455aac39517a9b295420 |
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| Source note | uspto-grants-2013_08 |
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