HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 58550238, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2-Piperidone | HCID 12665 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Benzyl bromoacetate | HCID 62576 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58550238 | HCID 58550238 | 24.5% |
Reaction Steps
Under a nitrogen atmosphere, to a solution of piperidin-2-one (9.8 g, 99 mmol) in N,N-dimethylformamide (100 ml) was added sodium hydride (4.4 g, 110 mmol) under ice-cooling, and the mixture was stirred for 1 hr. Then, benzyl bromoacetate (19 ml, 120 mmol) was added, and the mixture was further stirred for 2 hr. To the reaction mixture were added ethyl acetate and water, and the organic layer was separated, washed successively with water and saturated brine, and dried over sodium sulfate. Sodium sulfate was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography to give the title compound (6.0 g, yield 24%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299070B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-14ef7ff3cd4f4eb6aa30df3a9c5290b8 |
| Source note | uspto-grants-2012_10 |