HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl 4-oxopiperidine-1-carboxylate → Tert-butyl 4-[(2-ethoxy-2-oxoethyl)amino]piperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| Reactant | Glycine ethyl ester, hydrochloride | HCID 2723640 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Tert-butyl 4-[(2-ethoxy-2-oxoethyl)amino]piperidine-1-carboxylate | HCID 15380724 | 83.5% |
Reaction Steps
Sodium cyanoborohydride (189 mg, 3.01 mmol) was added to a solution of 1-boc-4-piperidone (500 mg, 2.51 mmol) and glycine ethyl ester hydrochloride (350 mg, 2.51 mmol) in methanol (12.5 mL). After 16 h, the mixture was quenched with saturated ammonium chloride solution, concentrated, and partitioned between dichloromethane and saturated sodium bicarbonate solution. The organic layer was washed with brine, dried over magnesium sulfate, filtered, and concentrated. Purification by silica gel chromatography [100% dichloromethane→95% dichloromethane/5% (10% ammonium hydroxide/methanol)] gave the title compound (600 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07947678B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-e9738eed29e54545ac7c85e18e816c0e |
| Source note | uspto-grants-2011_05 |