Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| Reactant | HCID 58313154 | HCID 58313154 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58313168 | HCID 58313168 | — |
Reaction Steps
To a solution of 7-ethyl 6-(phenylmethyl) 2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-6-azaspiro[3.4]octane-6,7-dicarboxylate (151) (1.87 g, 4.2 mmol) in THF (20 mL) was added glacial acetic acid (0.48 mL), followed by TBAF (8.5 mL, 1M solution in THF) and the reaction heated to 45° C. for 18 h. The reaction was concentrated in vacuo and partitioned between EtOAc and water. The organic layer was washed with saturated NaHCO3 followed by brine, and then dried over MgSO4 and concentrated in vacuo to afford the title compound as a clear oil in quantitative yield. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.17-7.48 (m, 5H) 4.83-5.15 (m, 3H) 3.88-4.34 (m, 4H) 3.35-3.47 (m, 2 H) 2.02-2.39 (m, 3H) 1.65-1.96 (m, 3H) 1.00-1.22 (m, 3H). LC-MS ESI (M+H)+=334.17.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08853416B2 |
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| Source dataset | uspto-grants-2014_10 |
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| ORD ID | ord-70907506917045abbff098699b13143e |
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| Source note | uspto-grants-2014_10 |
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