Hydrochloric Acid → HCID 610239, Verbindung

HRID 1264352Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1264352
[C:1]([C:5]1[CH:12]=[CH:11][C:8]([CH:9]=O)=[CH:7][CH:6]=1)([O:3][CH3:4])=[O:2].[C:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:15])[CH3:14].C[O-].[Na+].Cl>CO.CCOC(C)=O>[CH3:4][O:3][C:1](=[O:2])[C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH:14][C:13](=[O:15])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:7][CH:6]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 7410AcetophenoneHCID 15294Methyl 4-FormylbenzoateHCID 10942334Sodium Methoxide

Produkt 1

HCID 610239HCID 610239, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To 4-carbomethoxybenzaldehyde (79 mg, 0.48 mmol) and acetophenone (56 μL, 0.48 mmol) in anhydrous methanol (1.6 mL), was added neat sodium methoxide (26 mg, 0.48 mmol). The mixture was stirred at room temperature overnight then heated to reflux for 1 hour, cooled down to room temperature and added HCl 1N and EtOAc. The layers were separated and the organic layer dried over anhydrous MgSO4 and filtered. The solvent was evaporated under vacuum to afford a yellow solid, which was recrystallized from acetonitrile/water to give a pale yellow crystalline solid.

Aufarbeitung

  1. temperaturethen heated
  2. temperatureto reflux for 1 hour
  3. temperaturecooled down to room temperature
  4. customThe layers were separated
  5. dry with materialthe organic layer dried over anhydrous MgSO4
  6. filtrationfiltered
  7. customThe solvent was evaporated under vacuum
  8. customto afford a yellow solid, which
  9. customwas recrystallized from acetonitrile/water
  10. customto give a pale yellow crystalline solid

Quellen und Nachweise

ORD-Eintrag
ord-c32477a108304975971651b873999b78
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06541661B1

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