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Hydrochloric Acid → Piperazine-2,6-dione hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Benzylpiperazine-2,6-dione | HCID 560967 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol--water (1/1) | HCID 22242641 | — |
| 生成物 | Piperazine-2,6-dione hydrochloride | HCID 12476478 | — |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383621B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-17b8cbde4c364d3bac9328c7f2a81fd6 |
| 出典メモ | uspto-grants-2013_02 |