[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]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.
Wird geladen…
