3,4-dihydro-2H-pyran → HCID 19969552, Verbindung

HRID 974859Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 974859
O.C1(C)C(S(O)(=O)=O)=CC=CC=1.[CH2:13]([O:15][C:16]([CH:18]1[NH:23][C:22](=[O:24])[CH:21]([CH2:25][CH:26]([CH3:28])[CH3:27])[N:20]([OH:29])[C:19]1=[O:30])=[O:17])[CH3:14].[O:31]1[CH:36]=[CH:35][CH2:34][CH2:33][CH2:32]1>ClCCl>[CH2:13]([O:15][C:16]([CH:18]1[NH:23][C:22](=[O:24])[CH:21]([CH2:25][CH:26]([CH3:27])[CH3:28])[N:20]([O:29][CH:32]2[CH2:33][CH2:34][CH2:35][CH2:36][O:31]2)[C:19]1=[O:30])=[O:17])[CH3:14]

Komponenten

5

Edukt 3

HCID 80803,4-dihydro-2H-pyranHCID 124969952-Methylbenzenesulfonic acid hydrateHCID 19969538HCID 19969538, Verbindung

Produkt 1

HCID 19969552HCID 19969552, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

0.45 g of p, toluenesulfonic acid hydrate was added to 60 ml of a solution of 6.15 g of 3-ethoxycarbonyl-1-hydroxy-6-isobutylpiperazine-2,5-dione and 4 ml of 3,4-dihydro-2H-pyran in anhydrous dichloromethane. The mixture was stirred at room temperature for 4 hours. The reaction mixture was washed with an aqueous solution saturated with sodium hydrogen carbonate and then dried with anhydrous magnesium sulfate. The resulting mixture was subjected to distillation to remove the solvent to obtain 9.67 g of 3-ethoxycarbonyl-6-isobutyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione as an orange oily substance.

Aufarbeitung

  1. washThe reaction mixture was washed with an aqueous solution saturated with sodium hydrogen carbonate
  2. dry with materialdried with anhydrous magnesium sulfate
  3. distillationThe resulting mixture was subjected to distillation
  4. customto remove the solvent

Quellen und Nachweise

ORD-Eintrag
ord-2ab6faded25340c787eb799c4fb870e9
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05607934

Notizen zur Reaktion

Wird geladen…