Hydrochloric Acid → Piperazine-2,6-dione hydrochloride

HRID 389985

Reaktionsgleichung

Reaktionsgleichung von HRID 389985
C([N:8]1[CH2:13][C:12](=[O:14])[NH:11][C:10](=[O:15])[CH2:9]1)C1C=CC=CC=1.[ClH:16]>CO.O.CO.[Pd]>[ClH:16].[NH:11]1[C:12](=[O:14])[CH2:13][NH:8][CH2:9][C:10]1=[O:15]

Komponenten

6

Edukt 2

HCID 313Hydrochloric AcidHCID 5609674-Benzylpiperazine-2,6-dione

Produkt 1

HCID 12476478Piperazine-2,6-dione hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 23938PalladiumLösungsmittelHCID 22242641Methanol--water (1/1)Lösungsmittel

Versuchsvorschrift

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%).

Aufarbeitung

  1. customThe reaction mixture was degassed 3 times with hydrogen/vacuum
  2. filtrationThe reaction mixture was then filtered on Clarcel®
  3. washwashed with methanol
  4. concentrationThe filtrate was finally concentrated to dryness
  5. customthe residue was precipitated from a mixture of methanol and ether

Quellen und Nachweise

ORD-Eintrag
ord-17b8cbde4c364d3bac9328c7f2a81fd6
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08383621B2

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