Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Iodopropane | HCID 33643 | — |
| Reactant | 1-Tert-butyl 4-ethyl piperidine-1,4-dicarboxylate | HCID 2758812 | — |
| Reactant | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 46318390 | HCID 46318390 | 66.5% |
Reaction Steps
To a solution of potassium hexamethyldisilazide (29.1 g, 146 mmol) in THF (200 mL) at −78° C. was added ethyl N-Boc-piperidine-4-carboxylate (25 g, 97 mmol). The reaction mixture was stirred at −78° C. for 30 minutes, then 1-iodopropane (14.2 mL, 146 mmol) was slowly added. The reaction mixture was stirred at −78° C. for a further 20 minutes, then warmed to room temperature and stirred for 1 hour. The reaction was quenched by addition of saturated aqueous NH4Cl solution and extracted with EtOAc. The combined organic extracts were washed with brine, dried over MgSO4, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography (0% to 50% EtOAc in hexanes) to afford 19.3 g (66%) of 4-propyl-piperidine-1,4-dicarboxylic acid 1-tert-butyl ester 4-ethyl ester as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08513425B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-3e13ba24bc7345b9acf1be8d62be8b3d |
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| Source note | uspto-grants-2013_08 |
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