反应详情

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.

1. custom(temperature rise to 50° C.)
2. filtrationThe mixture is filtered with suction through a glass frit at 20° C.
3. customthe phases are separated
4. customthe organic phase is evaporated
5. customThe residue is recrystallized from methyl tert.-butyl ether
6. custom32.9 g of the above compound of melting point 66°-68° C., identical with a product prepared
7. customare obtained