Compound having allyl and propanohydrazide pyrimidine structure at terminal, preparation method and application of compound
A compound, pyrimidine technology, applied in the field of medicine, can solve problems such as limited application
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Embodiment 1
[0020] The synthesis of embodiment 1 compound I-1
[0021]
[0022] Step 1. Synthesis of Compound VI-1
[0023] Compound II (1.32g, 20mmol) was dissolved in 20mL DMSO, stirred at room temperature, KOH solid (2.24g, 40mmol) was added, and stirred at room temperature for 1 hour. Further MeI (III-1, 2.84 g, 20 mmol) was added, and stirring was continued overnight at room temperature. Then tert-butyl acrylate V-1 (2.56 g, 20 mmol) was added, and the stirring was continued for 12 hours, and TLC detection found that the reaction was complete.
[0024] The reaction mixture was carefully poured into 200mL ice water, stirred, and washed with 50mL×3CH 2 Cl 2 After extraction, the extract phases were combined, washed with 100 mL of 5% brine, and dried over anhydrous sodium sulfate. The desiccant was removed by suction filtration, the filtrate was evaporated to dryness on a rotary evaporator, and the residue was purified by silica gel column chromatography to obtain compound VI-I,...
Embodiment 2
[0031] The synthesis of embodiment 2 compound 1-2
[0032]
[0033] Step 1. Synthesis of compound VI-2
[0034]Compound II (1.32g, 20mmol) was dissolved in 20mL DMSO, stirred at room temperature, KOH solid (2.24g, 40mmol) was added, and stirred at room temperature for 1 hour. Another 20 mmol of compound III-2 was added, and stirring was continued overnight at room temperature. Then 20 mmol of compound V-2 was added, and the stirring was continued for 12 hours, and TLC detection found that the reaction was complete. The reaction mixture was carefully poured into 200mL ice water, stirred, and washed with 50mL×3CH 2 Cl 2 After extraction, the extract phases were combined, washed with 100 mL of 5% brine, and dried over anhydrous sodium sulfate. The desiccant was removed by suction filtration, the filtrate was evaporated to dryness on a rotary evaporator, and the residue was purified by silica gel column chromatography to obtain compound VI-2. ESI-MS, m / z=249 ([M+H] + )....
Embodiment 3
[0039] The synthesis of embodiment 3 compound 1-3
[0040]
[0041] Step 1. Synthesis of compound VI-3
[0042] Compound II (1.32g, 20mmol) was dissolved in 20mL DMSO, stirred at room temperature, KOH solid (2.24g, 40mmol) was added, and stirred at room temperature for 1 hour. Another 20 mmol of compound III-2 was added, and stirring was continued overnight at room temperature. Then 20 mmol of compound V-3 was added, and the stirring was continued for 12 hours, and TLC detection found that the reaction was complete. The reaction mixture was carefully poured into 200mL ice water, stirred, and washed with 50mL×3CH 2 Cl 2 After extraction, the extract phases were combined, washed with 100 mL of 5% brine, and dried over anhydrous sodium sulfate. The desiccant was removed by suction filtration, the filtrate was evaporated to dryness on a rotary evaporator, and the residue was purified by silica gel column chromatography to obtain compound VI-3. ESI-MS, m / z=263 ([M+H] + )...
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