* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
EXAMPLE 2 2-Amino-4-methoxy-6-methyl-s-triazine To a 100 ml. flask charge 5.5 gm. acetamidine hydrochloride, 5.7 gm. dimethyl (N-cyanoimido)carbonate, 11 gm. methanol and 11 gm. toluene. Cool the mixture to 5° C. and add dropwise 11.8 gm. of 30percent sodium methoxide while maintaining the reaction temperature at 5°-10° C. When the addition is complete, warm the reaction mixture to room temperature. Filter the slurry and wash the filter cake with methanol. Reslurry the filtercake in water, filter, wash the filter cake with water. Dry the solids to give 6.1 gm. (87percent) 2-amino-4-methoxy-6-methyl-s-triazine, mp256°-258° C.
1,095 g (97.7%)
EXAMPLE 10 A mixture of 1,441 g (8 moles) of 30percent technical grade methanolic sodium methylate solution (BASF AG) and 2,150 ml of methanol was cooled to 0° C. 984.8 g (4 moles) of pure O-methylisourea sulfate (O-methylisourea sulfate, pure from SKW Trostberg AG) were added to this cooled solution, while stirring vigorously and with exclusion of atmospheric moisture, and the mixture was cooled at 0° C. for a further 15 minutes. 897 g (8 moles) of pure N-cyanoacetimido-ethyl ester were then added dropwise, while stirring and cooling externally (ice bath), such that the internal temperature did not rise above 6° C. When the addition of the N-cyanoacetimido-ethyl ester had ended, the mixture was stirred at an internal temperature of 0° C. for a further 2 hours. Thereafter, the reaction mixture was stirred at room temperature, without external cooling, for 22 hours and then cooled to 12° C. and centrifuged. To remove the sodium sulfate, the solid residue was suspended in 4 liters of water and the suspension was centrifuged. The residue was suspended once again in 4 liters of water, the suspension was centrifuged and the centrifugate was washed free of sodium sulfate. It was dried at 80° C. in a vacuum drying cabinet. The yield was 1,095 g (97.7percent) of 2-amino-4-methoxy-6-methyl-s-triazine having a melting point of 262°-264° C. (decomposition).
If Y is hydrogen in the case of the employed arylsulfonamide of the formula II, preferred amines of the formula IV according to the process of the invention are the following:2-amino-4-methyl-6-methoxy-s-triazine,2-amino-4-methyl-6-methoxypyrimidine,2-amino-4-methyl-6-difluoromethoxypyrimidine,2-amino-4,6-dimethoxypyrimidine,2-amino-4,6-dimethoxy-s-triazine,2-amino-4,6-dimethylpyrimidine,2-amino-4-methoxy-6-ethoxy-s-triazine,2-amino-4-dimethylamino-6-methoxy-s-triazine,2-amino-4-cyclopropyl-6-methoxy-s-triazine,...
16
[ 74223-64-6 ]
[ 57683-71-3 ]
[ 1668-54-8 ]
methyl 2-[[[[(4-hydroxy-6-methyl-1,3,5-triazine-2-yl)amino]carbonyl]amino]sulfonyl]benzoate[ No CAS ]
methyl 2-[[[[[[[(acetylamino)carbonyl]amino]carbonyl]amino]carbonyl]amino]sulfonyl]benzoate[ No CAS ]
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