Unsaturated hydrocarbon pyrimidine sulfoether compound as well as preparation method and application thereof
A kind of technology of pyrimidine sulfide and compound, which is applied in the field of unsaturated hydrocarbon pyrimidine sulfide compound and preparation thereof, and can solve the problems such as unsatisfactory effect and the like
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Embodiment 1
[0133] Embodiment 1: the synthesis of compound 81
[0134] (1) Synthesis of intermediate 3a
[0135]
[0136] Slowly add 26.4g (0.48mol) of sodium methoxide in methanol solution dropwise to 18.24g (0.24mol) of thiourea in 150ml of methanol solution under stirring at room temperature, and continue stirring at room temperature for 2h after dropping. Then 26 g (0.2 mol) of ethyl acetoacetate was added dropwise to the above solution, and the reaction was stirred under reflux for 6-8 hours. After the reaction was detected by TLC, the solvent was evaporated under reduced pressure, the pH was adjusted to 5-6 with hydrochloric acid, and a solid was precipitated, which was filtered with suction to obtain a white solid, and dried to obtain 27 g of a white solid. Yield 95%.
[0137] (2) Synthesis of intermediate 5a
[0138]
[0139] Dissolve 1.42g (0.01mol) of 3a in 15ml of N,N-dimethylformamide, add 1.51g of potassium carbonate, stir for 0.5h, add 1.9g of 4a dropwise, raise the...
Embodiment 2
[0143] Embodiment 2: the synthesis of compound 258
[0144] (1) Synthesis of intermediate 3c
[0145] Dissolve 1.78g (0.01mol) of 1c in 15ml of N,N-dimethylformamide, add 1.51g of potassium carbonate, stir for 0.5h, add 1.2g of 2c dropwise, raise the temperature to 60°C after dropping, and stir for 4h . After the reaction was detected by TLC, the solvent was evaporated under reduced pressure, water was added and hydrochloric acid was added to adjust the pH to 5-6, a solid was precipitated, and a white solid was obtained by suction filtration and dried to obtain 2.2 g of a white solid. Yield 86.9%.
[0146]
[0147] (2) Synthesis of Compound 258
[0148] Dissolve 1.3g (0.005mol) of 3c in 10ml of N,N-dimethylformamide, add 0.83g of potassium carbonate, stir for 0.5h, add 1.45g of 2b in batches, heat up to 80°C after addition, and stir for 8h . After the reaction was detected by TLC, the reaction solution was poured into 50 ml of saturated saline, extracted three times wi...
Embodiment 3
[0150] Embodiment 3: the synthesis of compound 315
[0151] Dissolve 1.35g (0.005mol) of 1b in 10ml of N,N-dimethylformamide, add 0.83g of potassium carbonate, stir for 0.5h, add 1.45g of 2b in batches, heat up to 80°C after addition, and stir for 8h . After the reaction was detected by TLC, the reaction solution was poured into 50 ml of saturated saline, extracted three times with 100 ml of ethyl acetate, and dried. After precipitation, it was purified by column chromatography using petroleum ether: ethyl acetate 1000:1-300 eluent to obtain 1.92 g of an oily product.
[0152]
PUM
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