Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | 1-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid | HCID 392871 | — |
| Reactant | HCID 178504810 | HCID 178504810 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 25026509 | HCID 25026509 | — |
Reaction Steps
To a solution of piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (2.06 g, 9 mmol), NEt3 (1.2 g, 12 mmol) in toluene (150 mL) was added isobutylchloroformate (1.23 g, 9 mmol) at 0° C. The mixture was stirred at room temperature for 1.5 hours. N-hydroxy-2-(4-methanesulfonyl-phenoxy)-acetamidine (1.5 g, 6 mmol) was added to the mixture. The mixture was heated under reflux overnight, cooled and the mixture was washed successively with H2O and brine. After drying (Na2SO4), the solvent was removed. The residue was purified by flash chromatography on silica gel to afford the desired product. 1H NMR (CDCl3): δ 7.98 (2H, m), 7.14 (2H, m), 5.24 (2H, s), 4.2-4.05 (2H, m), 3.14 (1H, m), 3.03 (3H, s), 2.95 (2H, m), 2.12˜2.04 (2H, m), 1.80 (2H, m), 1.46 (9H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08975258B2 |
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| Source dataset | uspto-grants-2015_03 |
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| ORD ID | ord-b0522b8a0d7447dbae006f7f520346e5 |
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| Source note | uspto-grants-2015_03 |
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