HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 86729355, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| Reactant | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86729355 | HCID 86729355 | — |
Reaction Steps
To a solution of MeI (1.4 g, 10 mmol) in DMF was added NaH (0.40 g, 10 mmol, 60% in mineral oil), followed by diethyl (cyanomethyl)phosphonate (2.3 g, 10 mmol). The mixture was stirred at ambient temperature. After 30 minutes another batch of NaH (0.40 g, 10 mmol, 60% in mineral oil) was added, followed by tert-butyl 4-oxopiperidine-1-carboxylate (2.0 g, 10 mmol). The resulting mixture was stirred for 30 minutes before the reaction was quenched with water and the mixture was concentrated in vacuo. The crude residue was purified by MPLC on silica gel to afford the title compound. LRMS (ESI) calc'd for C13H21N2O2 [M+H]+237. Found 237.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09328099B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-b7273614e8d14973b48ae59d22101cb3 |
| Source note | uspto-grants-2016_05 |