[Br:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[NH:6][CH:7]=1.[O:9]1[CH:11]([C:12]([Cl:15])([Cl:14])[Cl:13])[CH2:10]1.C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[OH:9][CH:11]([C:12]([Cl:15])([Cl:14])[Cl:13])[CH2:10][N:4]1[CH:3]=[C:2]([Br:1])[CH:7]=[N:6][C:5]1=[O:8]A stirred mixture of 5-bromopyrimid-2-one (0.009 mol), 1,2-epoxy-3,3,3-trichloropropane (0.009 mol) and K2CO3 (33 mg) in dimethylformamide (40 ml ) was heated at 80° C. for 4 h. The reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg). The crystalline residue was triturated with a little ether and dissolved in ethyl acetate. The filtered ethyl acetate solution was concentrated to about 50 ml and left in the cold when the product crystallized out in 52% yield. m.p. 210°-212° C. (ethyl acetate).
Wird geladen…