Aluminum(III) Chloride → 6-(3-Carbomethoxy-2-methyl-propionyl)-3,4-dihydro-2(1H)-quinazolinone

HRID 1164794

Reaktionsgleichung

Reaktionsgleichung von HRID 1164794
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][NH:3][C:2]1=[O:11].[Cl-].[Al+3].[Cl-].[Cl-].[C:16]([CH2:20][CH:21]([CH3:25])[C:22](Cl)=[O:23])([O:18][CH3:19])=[O:17]>C(=S)=S>[C:16]([CH2:20][CH:21]([CH3:25])[C:22]([C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[NH:1][C:2](=[O:11])[NH:3][CH2:4]2)=[O:23])([O:18][CH3:19])=[O:17]

Komponenten

5

Edukt 3

HCID 6451240Aluminum(III) ChlorideHCID 123607563,4-Dihydroquinazolin-2(1H)-oneHCID 14403282Methyl 4-chloro-3-methyl-4-oxobutanoate

Produkt 1

HCID 146206376-(3-Carbomethoxy-2-methyl-propionyl)-3,4-dihydro-2(1H)-quinazolinone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6348Carbon DisulfideLösungsmittel

Versuchsvorschrift

3,4-Dihydro-2(1H)-quinazolinone (3.6 g) is added to a stirred suspension of anhydrous aluminum chloride (16.5 g) in carbon disulfide (120 ml) under nitrogen. 3-Carbomethoxy-2-methyl-propionyl chloride (4 g) is added dropwise to the stirred suspension, and the reaction mixture refluxed for about 18 hours, cooled to RT and further cooled to 0° C. in an ice bath. The liquid phase is decanted and ice and cold water slowly added to the residue. The aqueous mixture is filtered and the filtered solid suspended and stirred in the anhydrous diethyl ether overnight. The suspension is filtered and the filtered solid used in the next step without further purification.

Aufarbeitung

  1. temperaturethe reaction mixture refluxed for about 18 hours
  2. temperaturefurther cooled to 0° C. in an ice bath
  3. customThe liquid phase is decanted
  4. additionice and cold water slowly added to the residue
  5. filtrationThe aqueous mixture is filtered
  6. filtrationThe suspension is filtered
  7. customthe filtered solid used in the next step without further purification

Quellen und Nachweise

ORD-Eintrag
ord-75509c6ccdda4ccba40ecc7c56b9bd22
Quelldatensatz
uspto-grants-1990_03
Patentnummer
US04906630

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