Benzyl 4-(2-hydroxy-2-methylpropionyl)piperazine-1-carbamate → 2-Hydroxy-2-methyl-1-(piperazin-1-yl)propan-1-one
Reaktionsgleichung
[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
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
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
- customthe reaction system was purged with hydrogen at atmospheric pressure
- customAfter the reaction system was purged with nitrogen
- filtrationthe catalyst was filtered out
- washwashed with methanol
- distillationthe solvent, together with the filtrate and the washing solution, was distilled off
- 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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