A kind of preparation method of 2-methyl-4-amino-6-chloropyrimidine
A technology of methylpyrimidine and chloropyrimidine, which is applied in the field of preparation of 2-methyl-4-amino-6-chloropyrimidine, can solve the problems of poor economic benefit and environmental impact, difficult reaction, complicated operation, etc., and achieve simplification Reaction process and post-treatment process, reduce production cost, optimize the effect of preparation process
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Embodiment 1
[0020] The first step: the synthesis of 4,6-dichloro-2-methylpyrimidine
[0021] 4,6-Dihydroxy-2-methylpyrimidine (5.0g, 0.04mol) was added to a mixed solution of phosphorus oxychloride (18.4g, 0.12mol) and acetonitrile, and the reaction was stirred at 60°C for 3 hours, and confirmed by spotting Raw material points disappear. The excess phosphorus oxychloride was distilled under reduced pressure, and the residue was poured into 50 g of ice water. The precipitated solid was filtered and purified by column to obtain 6 g (yield: 92%) of solid.
[0022] After nuclear magnetic detection, the nuclear magnetic spectrum is as follows, and the solid can be determined to be 4,6-dichloro-2-methylpyrimidine.
[0023] 1H NMR (CDCl3, 400MHz): d 2.63 (s, 3H, CH3), 7.17 [s, 1H, H (5)].
[0024] The second step: the synthesis of 2-methyl-4-amino-6-chloropyrimidine
[0025] Add 4,6-dichloro-2-methylpyrimidine (50g, 0.31mol) and ammonia water (0.5L) into a 1L reaction flask, stir at 40°C fo...
Embodiment 2
[0030] The first step: the synthesis of 4,6-dichloro-2-methylpyrimidine
[0031] 4,6-dihydroxy-2-methylpyrimidine (5.0g, 0.04mol) was added to a mixed solution of phosphorus oxychloride (12.26g, 0.08mol) and acetonitrile, and the reaction was stirred at 70°C for 3 hours, and confirmed by spotting Raw material points disappear. The excess phosphorus oxychloride was distilled under reduced pressure, and the residue was poured into 50 g of ice water. The precipitated solid was filtered and purified by column to obtain 5.8 g (yield: 90%) of solid.
[0032] Through nuclear magnetic detection, the solid can be determined to be 4,6-dichloro-2-methylpyrimidine.
[0033] The second step: the synthesis of 2-methyl-4-amino-6-chloropyrimidine
[0034] Add 4,6-dichloro-2-methylpyrimidine (50g, 0.31mol) and a mixed solution of ammonia water and tetrahydrofuran (0.5L) into a 1L reaction flask, stir at 45°C for 5 hours, cool the reaction to room temperature, filter, and use Wash with petro...
Embodiment 3
[0038] The first step: the synthesis of 4,6-dichloro-2-methylpyrimidine
[0039] 4,6-dihydroxy-2-methylpyrimidine (5.0g, 0.04mol) was added to a mixed solution of thionyl chloride (18.9g, 0.16mol) and acetonitrile, and the reaction was stirred at 80°C for 3 hours, and confirmed by spotting Raw material points disappear. The excess thionyl chloride was distilled under reduced pressure, and the residue was poured into 50 g of ice water. The precipitated solid was filtered and purified by column to obtain 6.1 g (yield: 94%) of solid.
[0040] Through nuclear magnetic detection, the solid can be determined to be 4,6-dichloro-2-methylpyrimidine.
[0041] The second step: the synthesis of 2-methyl-4-amino-6-chloropyrimidine
[0042] Add 4,6-dichloro-2-methylpyrimidine (50g, 0.31mol) and methanolic ammonia solution (0.5L) into a 1L reaction flask, stir at 50°C for 5 hours, cool the reaction to room temperature, filter, and use petroleum Wash with ether (100ml), filter, and dry und...
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