[NH2:1][N:2]1[C:7](=[O:8])[C:6]([CH:9]([CH:11]2[CH2:13][CH2:12]2)[CH3:10])=[N:5][N:4]=[C:3]1[S:14][CH3:15].[CH3:16]I.[OH-].[Na+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH:11]1([CH:9]([C:6]2[C:7](=[O:8])[N:2]([NH:1][CH3:16])[C:3]([S:14][CH3:15])=[N:4][N:5]=2)[CH3:10])[CH2:12][CH2:13]1
100 ml of toluene and 56.5 g (0.25 mol) of 4-amino-6-(1-cyclopropylethyl)-3-methylthio-1,2,4-triazin-5(4H)-one, and then 89.5 g (0.63 mol) of methyl iodide and 8.5 g (0.025 mol) of tetrabutylammonium bromide are added to 100 ml of 50% strength aqueous sodium hydroxide solution with vigorous stirring. The emulsion is stirred vigorously until the exothermic reaction abates (temperature rise to 50° C.). The mixture is filtered with suction through a glass frit at 20° C., the phases are separated and the organic phase is evaporated. The residue is recrystallized from methyl tert.-butyl ether. 32.9 g of the above compound of melting point 66°-68° C., identical with a product prepared according to process A (cf. Example 5), are obtained.
Wird geladen…
