HCID 178418573, Verbindung → HCID 178441847, Verbindung

HRID 487054Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 487054
[CH2:1]([C:5]1[NH:6][C:7]2[C:12]([C:13](=[O:15])[N:14]=1)=[CH:11][C:10]([CH:16]=[O:17])=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH3:4].[CH3:18][Mg]Br>O1CCCC1.C(OCC)C>[CH2:1]([C:5]1[NH:6][C:7]2[C:12]([C:13](=[O:15])[N:14]=1)=[CH:11][C:10]([CH:16]([OH:17])[CH3:18])=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH3:4]

Komponenten

5

Edukt 2

HCID 178418573HCID 178418573, VerbindungHCID 178441857HCID 178441857, Verbindung

Produkt 1

HCID 178441847HCID 178441847, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of 0.60 g of 2-butyl-1,4-dihydro-4-oxo-6-quinazolinecarboxaldehyde in 30 ml of dry tetrahydrofuran, cooled to 0° C. is added dropwise, 2.61 ml of a 3.0M solution of methylmagnesium bromide in diethyl ether. The reaction is stirred at 0° C. for 30 minutes and then quenched with 10 ml of aqueous ammonium chloride. After diluting with 10 ml of water, the reaction mixture is extracted with 9:1 chloroform-methanol. The combined extracts are dried with magnesium sulfate, filtered and concentrated to yield 0.64 g of the desired product.

Aufarbeitung

  1. additionis added dropwise
  2. customquenched with 10 ml of aqueous ammonium chloride
  3. additionAfter diluting with 10 ml of water
  4. extractionthe reaction mixture is extracted with 9:1 chloroform-methanol
  5. dry with materialThe combined extracts are dried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-d2da8b328fa14a7c94cc7d2fd6e558d3
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05294611

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