Diethylamine → 3-(Boc-amino)piperidine

HRID 501411Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 501411
C(NCC)C.[C:6]([O:10][C:11]([NH:13][CH:14]1[CH2:19][CH2:18][CH2:17][N:16](C(OCC2C3C=CC=CC=3C3C2=CC=CC=3)=O)[CH2:15]1)=[O:12])([CH3:9])([CH3:8])[CH3:7]>C(O)C>[NH:16]1[CH2:17][CH2:18][CH2:19][CH:14]([NH:13][C:11](=[O:12])[O:10][C:6]([CH3:8])([CH3:7])[CH3:9])[CH2:15]1

Komponenten

4

Edukt 2

HCID 8021DiethylamineHCID 23070937HCID 23070937, Verbindung

Produkt 1

HCID 42330413-(Boc-amino)piperidineAusbeute 88,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

25 ml of diethylamine was added to 250 ml of an ethanol solution of 1.88 g of 9H-fluoren-9-ylmethyl 3-t-butoxycarbonylaminopiperidine-1-carboxylate, and the mixture was stirred at room temperature for 18 hours. After the solution had been concentrated under reduced pressure, the residue was dissolved in a mixture consisting of 150 ml of toluene and 100 ml of 10% aqueous citric acid solution. The aqueous layer was made alkaline with a 5N aqueous sodium hydroxide solution, and then extracted twice with 100 ml of dichloromethane. The organic layers were combined together, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give 0.79 g of the title compound.

Aufarbeitung

  1. concentrationAfter the solution had been concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in a mixture
  3. extractionextracted twice with 100 ml of dichloromethane
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d8aeda4238644949a7c71f8691229e49
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772226B2

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