6-aryl aminopyrimidine compound and synthetic method thereof
An arylaminopyrimidine and a synthesis method technology are applied in the field of 6-arylaminopyrimidine compounds and their synthesis, which can solve the problems of low efficiency, inability to meet high-throughput screening, difficulty in compound synthesis, and the like, and achieve high yield , to achieve the effect of molecular diversity and product stability
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Embodiment 1
[0059] Synthesis of 2-amino-6-p-chlorophenyl-4-methylthiopyrimidine (A): 5.1 grams of dry 1-p-chlorophenyl-3,3-dimethylsulfanyl was added successively in a 250 ml round-bottomed flask -Acrylone crystals, 14.4 grams of dry guanidine carbonate crystals, heated to 115° C. in an oil bath under stirring with a magnetic stirrer, reacted for 4 hours and the mixture turned into a yellow powder, and the TLC spot plate detection reaction was complete, and the reaction was stopped, and the resulting yellow powder was Washed twice with 50 ml of hot water, filtered while hot, and dried naturally, yield 98%, melting point: 140°C-141°C. 1 H NMR (500MHz, CDCl 3 )δppm: 2.54 (3H, S-CH 3 ), 5.29 (2H, NH2); 13 C NMR (125MHz, CDCl 3 )δppm: 12.8, 77.4, 129.3, 162.5, 172.4. ESI-MS for C 11 h 10 ClN 3 S Calcd.251.0362 (M + ); Found: 252.0503(M + +H).
Embodiment 2
[0061] Synthesis of 2-amino-6-phenyl-4-methylthiopyrimidine (B): 5.55 g of dry 1-phenyl-3,3-dimethylthio-propenone were successively added to a 250 ml round bottom flask Crystals, 14.4 grams of dry guanidine carbonate crystals were heated to 115° C. with an oil bath under magnetic stirrer stirring, and the mixture became a yellow powder after 4 hours of reaction. The TLC spot plate detection reaction was complete, and the reaction was stopped. The resulting yellow powder was mixed with 50 ml Washing with hot water twice, suction filtration while hot, air-drying, the yield is 90%, melting point: 114°C-115°C. 1 H NMR (500MHz, CDCl 3 )δppm: 2.46 (3H, S-CH 3 ), 4.98 (2H, NH2); 13 C NMR (125MHz, CDCl 3 )δppm: 12.8, 77.4, 129.0, 162.8, 172.1. ESI-MS for C 11 h 11 N 3 S Calcd.217.0674 (M + ); Found: 218.0881(M + +H).
Embodiment 3
[0063] Synthesis of 2-amino-6-p-methylphenyl-4-methylthiopyrimidine (D): 5.1 grams of dry 1-p-methylphenyl-3,3-di Methylthio-propenone crystals, 14.0 grams of dry guanidine carbonate crystals, heated to 115° C. with an oil bath under stirring with a magnetic stirrer, reacted for 4 hours and the mixture turned into a yellow powder, and the TLC spot plate detection reaction was complete, and the reaction was stopped. The obtained yellow powder was washed twice with 50 milliliters of hot water, suction filtered while it was hot, and dried naturally, with a yield of 82%.
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