HCID 69622564, Verbindung → HCID 14110361, Verbindung

HRID 1826128Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1826128
ClC(Cl)(Cl)COC([N:7]1[C:13]2[CH:14]=[CH:15][C:16]([O:18][CH3:19])=[CH:17][C:12]=2[C:11](=[O:20])[N:10]2[CH2:21][CH2:22][CH2:23][C@H:9]2[C@@H:8]1O)=O>C1COCC1.CCOC(C)=O>[CH3:19][O:18][C:16]1[CH:15]=[CH:14][C:13]2[N:7]=[CH:8][CH:9]3[CH2:23][CH2:22][CH2:21][N:10]3[C:11](=[O:20])[C:12]=2[CH:17]=1

Komponenten

4

Edukt 1

HCID 69622564HCID 69622564, Verbindung

Produkt 1

HCID 14110361HCID 14110361, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

10% Cd/Pb couple (2.50 g, 20 mmol Cd) was added to a rapidly stirring solution of 95 (1.71 g, 4.03 mmol) in a mixture of THF (30 mL) and 1N NH4OAc (30 mL). Upon addition, the solution turned cloudy and after 2 hours TLC showed the reaction to be complete. The reaction mixture was diluted with EtOAc (150 mL) and dried over anhydrous MgSO4. The solids were filtered and rinsed with EtOAc (50 mL). Removal of excess solvent by rotary evaporation under reduced pressure afforded the product as a yellow solid (0.84 g, 3.6 mmol, 90%).

Aufarbeitung

  1. additionUpon addition
  2. customthe reaction
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationThe solids were filtered
  5. washrinsed with EtOAc (50 mL)
  6. customRemoval of excess solvent
  7. customby rotary evaporation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-5df9be46ba67463c88d282146be37afa
Quelldatensatz
uspto-grants-2006_05
Patentnummer
US07049311B1

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