Theanine and RGDS co-modified 5-fluorouracil as well as synthesis, activity and application thereof
A fluorouracil and reaction technology, which can be used in medical preparations containing active ingredients, drug combinations, peptide/protein components, etc., and can solve problems such as failure to achieve expected effects.
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Embodiment 1
[0019] Embodiment 1 prepares Boc-Arg (NO 2 )-Gly-OBzl
[0020] 3.19g (10mmol) Boc-R(NO 2 ) was dissolved in anhydrous tetrahydrofuran (THF), and 1.35 g (10 mmol) of 1-hydroxybenzotriazole and 2.68 g (13 mmol) of dicyclohexylcarbodiimide were sequentially added to the resulting solution. After stirring for 30 min, 3.71 g (1.1 mmol) of Gly-OBzl in tetrahydrofuran was added to the reaction solution, and N-methylmorpholine was added dropwise to the reaction solution at 0°C to adjust the pH to 8. The reaction solution was stirred at room temperature until TLC showed that the reaction was complete. The reaction mixture was filtered, the filtrate was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate solution. Purification by silica gel column chromatography gave 3.53 g (75%) of the title compound as a colorless solid. ESI-MS(m / e): 467[M+H] + .
Embodiment 2
[0021] Example 2 Preparation of Boc-Asp(OBzl)-Ser-OBzl
[0022] Using the method of Example 1, 3.86g (77%) of the title compound was obtained as a colorless solid from 3.32g (10mmol) Boc-Asp(OBzl) and 2.78g (1.2mmol) Ser-OBzl. ESI-MS(m / e): 501[M+H] + .
Embodiment 3
[0023] Embodiment 3 prepares Boc-Arg (NO 2 )-Gly
[0024] 5.33g (5mmol) Boc-Arg(NO 2 )-Gly-OBzl was dissolved in methanol, and the pH value of the reaction solution was adjusted to 13 with sodium hydroxide solution (2M). Continue the reaction at 0°C until the reaction is complete as monitored by TLC. The pH of the reaction was adjusted to neutral with 2N hydrochloric acid solution. Concentrate under reduced pressure to remove methanol. Continue to add 2N hydrochloric acid solution dropwise at 0°C to adjust the pH value to 2. The solution was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride until neutral, and dried by adding anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure to remove the solvent to obtain 1.63 g (86%) of the title compound as a white solid. ESI-MS(m / e): 375[M-H] - .
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