4-Methylmorpholine → 1,4-Bis(tert-butoxycarbonyl)-2-formylmethylpiperazine

HRID 352831Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 352831
CN1CCOCC1.[C:8]([O:12][C:13]([N:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH:16]1[CH2:28][CH2:29][OH:30])=[O:14])([CH3:11])([CH3:10])[CH3:9]>C(Cl)Cl.[Ru]([O-])(=O)(=O)=O.C([N+](CCC)(CCC)CCC)CC>[C:8]([O:12][C:13]([N:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH:16]1[CH2:28][CH:29]=[O:30])=[O:14])([CH3:11])([CH3:10])[CH3:9]

Komponenten

5

Edukt 2

HCID 79724-MethylmorpholineHCID 22710988di-tert-Butyl 2-(2-hydroxyethyl)piperazine-1,4-dicarboxylate

Produkt 1

HCID 227100181,4-Bis(tert-butoxycarbonyl)-2-formylmethylpiperazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178419074HCID 178419074, VerbindungKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

In methylene chloride (150 ml) was dissolved 1,4-bis(tert-butoxycarbonyl)-2-(2-hydroxyethyl)piperazine. Under ice cooling, N-methylmorpholine (2.14 g) and tetra-n-propylammonium perruthenate (0.97 g) were added to the reaction mixture, followed by stirring at room temperature for 17 hours. The reaction mixture was then distilled off under reduced pressure. The residue was subjected to chromatography on a silica gel column (hexane:ethyl acetate=9:1 to 2:1), whereby the title compound (3.11 g) was obtained as colorless powder.

Aufarbeitung

  1. distillationThe reaction mixture was then distilled off under reduced pressure
  2. customwas obtained as colorless powder

Quellen und Nachweise

ORD-Eintrag
ord-e4e084b2d70246b787df9f9be46e0e48
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06747023B1

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