Benzyl 4-(2-hydroxy-2-methylpropionyl)piperazine-1-carbamate → 2-Hydroxy-2-methyl-1-(piperazin-1-yl)propan-1-one

HRID 2376835Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2376835
[OH:1][C:2]([CH3:23])([CH3:22])[C:3]([N:5]1[CH2:10][CH2:9][N:8](NC(OCC2C=CC=CC=2)=O)[CH2:7][CH2:6]1)=[O:4]>CO.[Pd]>[OH:1][C:2]([CH3:23])([CH3:22])[C:3]([N:5]1[CH2:6][CH2:7][NH:8][CH2:9][CH2:10]1)=[O:4]

Komponenten

4

Versuchsvorschrift

Benzyl 4-(2-hydroxy-2-methylpropionyl)piperazine-1-carbamate (2.82 g, 9.20 mmol) synthesized in Production example 28-1 was dissolved in methanol (100 ml) under nitrogen atmosphere; 10% palladium on carbon (50% wet, 1.96 g) was added thereto, the reaction system was purged with hydrogen at atmospheric pressure; and the reaction mixture was stirred overnight. After the reaction system was purged with nitrogen, the catalyst was filtered out, and washed with methanol, then the solvent, together with the filtrate and the washing solution, was distilled off. The residue was dried under reduced pressure to yield the title compound (1.58 g, 9.20 mmol, quantitative) as a colorless oil.

Aufarbeitung

  1. customthe reaction system was purged with hydrogen at atmospheric pressure
  2. customAfter the reaction system was purged with nitrogen
  3. filtrationthe catalyst was filtered out
  4. washwashed with methanol
  5. distillationthe solvent, together with the filtrate and the washing solution, was distilled off
  6. customThe residue was dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a013366a3c924a8ba798dfdf2aac4737
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07468380B2

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