9-(diethoxy) phosphonomethyl purine, preparation method and application thereof in antineoplastic aspect
A technology of diethoxy and adenine, which is applied in antineoplastic drugs, chemical instruments and methods, and pharmaceutical formulations, can solve problems in the initial stage and achieve the effect of easy operation
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Embodiment 1
[0032] (1) Synthesis of α-iodomethyl diethyl phosphate
[0033]Add diiodomethane (81mL, 1.00mol) into a 500mL three-necked flask equipped with a condensing side tube, heat to 110°C, the color of diiodomethane begins to darken, at this time slowly add triethyl phosphite, dropwise The temperature rises rapidly during the process, indicating that the reaction has begun. When the temperature rises to 140°C, the heat source is removed quickly, and the temperature is strictly controlled so that it cannot exceed 150°C. Triethyl phosphite (180mL, 1.05mol) is added dropwise until the reaction temperature begins. decrease, indicating that the reaction is complete. After complete cooling, a light yellow liquid was obtained. Distill it under reduced pressure at 13mmHg. When the temperature is 70-90°C, two fractions are distilled out successively. Then adjust the vacuum degree and distill under reduced pressure at 8mmHg. The temperature rises to 106°C, and the third fraction is distilled ...
Embodiment 2
[0037] (1) Synthesis of α-iodomethyl diethyl phosphate
[0038] Add diiodomethane (81mL, 1.00mol) into a 500mL three-necked flask equipped with a condensing side tube, heat to 110°C, the color of diiodomethane begins to darken, at this time slowly add triethyl phosphite, dropwise The temperature rises rapidly during the process, indicating that the reaction begins. When the temperature rises to 120°C, the heat source is removed quickly, and the temperature is strictly controlled so that it cannot exceed 130°C. Triethyl phosphite (180mL, 1.05mol) is added dropwise until the reaction temperature begins. decrease, indicating that the reaction is complete. After complete cooling, a light yellow liquid was obtained. Distill it under reduced pressure at 13mmHg. When the temperature is 70-90°C, two fractions are distilled out successively. Then adjust the vacuum degree and distill under reduced pressure at 8mmHg. The temperature rises to 106°C, and the third fraction is distilled ou...
Embodiment 3
[0042] (1) Synthesis of α-iodomethyl diethyl phosphate
[0043] Add diiodomethane (81mL, 1.00mol) into a 500mL three-necked flask equipped with a condensing side tube, heat to 100°C, the color of diiodomethane begins to darken, at this time slowly add triethyl phosphite, dropwise The temperature rises rapidly during the process, indicating that the reaction begins. When the temperature rises to 120°C, the heat source is removed quickly, and the temperature is strictly controlled so that it cannot exceed 130°C. Triethyl phosphite (180mL, 1.05mol) is added dropwise until the reaction temperature begins. decrease, indicating that the reaction is complete. After complete cooling, a light yellow liquid was obtained. Distill it under reduced pressure at 13mmHg. When the temperature is 70-90°C, two fractions are distilled out successively. Then adjust the vacuum degree and distill under reduced pressure at 8mmHg. The temperature rises to 106°C, and the third fraction is distilled ou...
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