HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → (3S)-1-Benzyl-3-ethylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | (S)-1-Benzyl-3-ethylpiperazine-2,5-dione | HCID 20598791 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (3S)-1-Benzyl-3-ethylpiperazine | HCID 17750461 | 99% |
Reaction Steps
A solution of 8.1 gm (34.9 mmol) 2(S)-ethyl-4-benzyl-3,6-dioxopiperazine in 50 mL tetrahydrofuran was added dropwise via addition funnel to a solution of 75 mL (75 mMol) lithium aluminum hydride (1M in tetrahydrofuran) and the mixture was heated at reflux for 2.5 h. The reaction was then cooled in an ice bath and was treated sequentially with 3 mL deionized water, 3 mL 5N sodium hydroxide, and 9 mL deionized water. The resulting slurry was allowed to stir for 1 hour and was then filtered. The recovered salts were rinsed with 100 mL tetrahydrofuran and 100 mL dichloromethane. The filtrate was concentrated in vacuo to afford 7.03 g (99%) of the desired piperazine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06638936B1 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-7ec84b5fdd3e4de2acd03db15d2521c0 |
| Source note | uspto-grants-2003_10 |