HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 1-tert-Butyl 4-ethyl 4-methylpiperidine-1,4-dicarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cyclohexane | HCID 8078 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Reactant | 1-Tert-butyl 4-ethyl piperidine-1,4-dicarboxylate | HCID 2758812 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-tert-Butyl 4-ethyl 4-methylpiperidine-1,4-dicarboxylate | HCID 16218276 | — |
Reaction Steps
A solution of Example 532A (2.1 g, 8.1 mmol) in THF (81 mL) at −78° C. was treated dropwise with 1.5M LDA in cyclohexane (6.0 mL, 8.9 mmol), stirred for 30 minutes, treated dropwise with methyl iodide (0.76 mL, 12.1 mmol), stirred for 2.5 hours, quenched with saturated NH4Cl, and extracted with diethyl ether. The combined extracts were washed with brine, dried (MgSO4), filtered and concentrated to provide the desired product. MS (DCI) m/e 272 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07504512B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-ce224a7eabf04ad5997f3efe1cb72212 |
| Source note | uspto-grants-2009_03 |