HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57516591, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | tert-Butyl (2-oxopiperidin-3-yl)carbamate | HCID 21260262 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57516591 | HCID 57516591 | 29% |
Reaction Steps
To a solution of tert-butyl(2-oxopiperidin-3-yl)carbamate (1714 mg) in DMF (20 mL) was added 60% sodium hydride (480 mg, containing mineral oil) under ice-cooling. The reaction mixture was stirred at room temperature for 30 min, and iodomethane (1703 mg) was added. The reaction mixture was stirred at room temperature overnight, water was added, and the mixture was extracted with ethyl acetate. The organic layer was separated, washed with water and saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (530 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772277B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-73b566ad2f4743628e9a895727fa18cb |
| Source note | uspto-grants-2014_07 |