HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 30720226, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 66935783 | HCID 66935783 | — |
| Product | HCID 30720226 | HCID 30720226 | 146.9% |
Reaction Steps
1M LAH in THF (3 mL, 3 mmol) was added dropwise to (3S,5S)-3,4,5-trimethyl-2-piperazinone (123 mg, 0.86 mmol). The reaction was allowed to warm to room temperature, then stirred at room temperature for 40 min and at reflux for an additional 5 h. After cooling to room temperature, the reaction was quenched by the sequential addition of H2O (0.114 mL), 15% NaOH (0.114 mL), and H2O (0.342 mL). The mixture was stirred for 0.5 h, and the solids were filtered off and washed with excess THF. To the combined filtrates was added 1.8 mL 1N HCl, followed by concentration under reduced pressure to provide the hydrochloride salt of (2S,6S)-1,2,6-trimethylpiperazine (162 mg, 93%). LCMS: (M+H)+: 129.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07893056B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-e1fa611b658d4785983e34d97dbbde0d |
| Source note | uspto-grants-2011_02 |