Methanol → HCID 178471115, Verbindung

HRID 657169Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 657169
[Na].[CH:2]([CH:4]([CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:5]([O:7]CC)=O)=O.[C:17]1(/[CH:23]=[CH:24]/[C:25](=[NH:27])[NH2:26])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.CO>CCO>[OH:7][C:5]1[C:4]([CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:2][N:27]=[C:25](/[CH:24]=[CH:23]/[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:26]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 14668188CinnamimidamideHCID 86635375Diethyl alpha-formylglutarate Sodium Salt

Produkt 1

HCID 178471115HCID 178471115, VerbindungAusbeute 59,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Diethyl α-formylglutarate sodium salt (1 g, 4.2 mmol) and (2E)-3-phenyl-2-propenimidamide (0.61 g, 4.2 mmol), prepared in Example 126 (g), were combined in EtOH (20 mL) and MeOH (10 mL) and heated at reflux for 12 h. The solvent was removed and the resulting solid triturated with ether and filtered to give the desired product as a yellow solid (0.75 g, 56%). The mother liquor contained additional product which was not isolated. LCMS (ES+) m/z 299 (MH+).

Aufarbeitung

  1. temperatureat reflux for 12 h
  2. customThe solvent was removed
  3. customthe resulting solid triturated with ether
  4. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-acd65e24c48e471eae398574b5eef723
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08071592B2

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