HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Piperazine-2,6-dione hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Benzylpiperazine-2,6-dione | HCID 560967 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Palladium | HCID 23938 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | Piperazine-2,6-dione hydrochloride | HCID 12476478 | — |
Reaction Steps
To a solution of 4-benzylpiperazine-2,6-dione (which may be prepared in accordance with the experimental described in Example 4, step 1; 2.0 g, 9.8 mmol) in a mixture of methanol/H2O (65 mL/28 mL) were added a solution of HCl 1N in methanol (23.8 mL) and Pd/C (10% wet, 0.2% wt., 400 mg). The reaction mixture was degassed 3 times with hydrogen/vacuum prior to its overnight stirring under hydrogen (P=1 atm). The reaction mixture was then filtered on Clarcel® and washed with methanol. The filtrate was finally concentrated to dryness and the residue was precipitated from a mixture of methanol and ether. The title product was obtained as a beige solid (418 mg, 28%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08383621B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-17b8cbde4c364d3bac9328c7f2a81fd6 |
| Source note | uspto-grants-2013_02 |