A compound for optical imaging, preparation method and bond thereof
A technology of optical imaging and compounds, applied in the field of optical imaging, can solve problems such as light energy loss, and achieve the effects of low cost, simple preparation method, and wide application
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[0051] The invention provides a preparation method of a compound for optical imaging, comprising:
[0052] A compound having a structure of formula a, 3-mercaptopropionic acid and triethylamine are subjected to a nucleophilic substitution reaction in a solvent to obtain a compound for optical imaging having a structure shown in formula I:
[0053]
[0054] M in formula I is selected from chloride ion or p-toluenesulfonate ion;
[0055]
[0056]In the present invention, the temperature of the nucleophilic substitution reaction between the compound of formula a, 3-mercaptopropionic acid and triethylamine is preferably 10°C to 30°C, more preferably 15°C to 25°C, most preferably 18°C ~22°C. In the present invention, the time for the nucleophilic substitution reaction of the compound of formula a, 3-mercaptopropionic acid and triethylamine is preferably 15 hours to 25 hours, more preferably 18 hours to 22 hours, most preferably 20 hours . In the present invention, the nucl...
Embodiment 1
[0107] Mix IR830 having the structure shown in formula b in a mixed solution of isopropanol and hydrochloric acid at 20°C for 10 minutes, then recrystallize, collect the solid, and dry it in vacuo to obtain the chloride salt of IR830 having the structure shown in formula a; moles of IR830 and hydrochloric acid The ratio is 1:50.
[0108] In the dry reaction bottle, add 1mmol of IR830 chloride salt, nitrogen protection, add 10mL of dimethylformamide (DMF), stir to dissolve, add 1.5mmol of triethylamine, 1.5mmol of 3-mercaptopropionic acid , 20°C sealed and protected from light for 20 hours. After the reaction, the obtained reaction product was settled with ethyl acetate, the solid was collected, and vacuum-dried at room temperature. The obtained dry product was redissolved with dichloromethane, and the obtained solution was saturated with Washing with salt water three times, drying the washed product with anhydrous sodium sulfate, filtering off the solid insoluble matter, conce...
Embodiment 2
[0114] Mix IR830 having the structure shown in formula b in a mixed solution of isopropanol and hydrochloric acid at 20°C for 10 minutes, then recrystallize, collect the solid, and dry it in vacuo to obtain the chloride salt of IR830 having the structure shown in formula a; moles of IR830 and hydrochloric acid The ratio is 1:50.
[0115] In a dry reaction flask, add 1 mmol of IR830 chloride salt, fill it with nitrogen, add 10 mL of DMF, stir to dissolve, add 1.2 mmol of triethylamine, 1.2 mmol of 4-aminothiophenol, seal at 0°C and avoid light Reacted for 20 hours, after the reaction was finished, the obtained reaction product was precipitated with ethyl acetate, the solid was collected, dried in vacuo at room temperature, the dried product was redissolved with dichloromethane, washed three times with saturated brine, and the washed product was After drying with anhydrous sodium sulfate, the solid insolubles were filtered off, the liquid obtained after filtration was concentrat...
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