A kind of reactive mercapto compound probe and preparation method thereof
A sulfhydryl compound and compound technology, applied in chemical instruments and methods, organic chemistry, fluorescence/phosphorescence, etc., can solve the problems of small capillary diameter, affecting separation reproducibility, difficult operation, etc., and achieve the effect of significant enhancement of fluorescence intensity.
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[0046] (1) Preparation of compound 1
[0047] Add 40 mL of toluene to a 150 mL round bottom flask, then add 11.0 g (0.1 mol) of resorcinol and 14.8 g (0.1 mol) of phthalic anhydride, stir to dissolve, stir and reflux for 5 hours, and gradually generate a solid, which is filtered off with suction The solid was recrystallized from methanol to obtain an orange solid.
[0048] The synthetic route is as follows:
[0049]
[0050] (2) Preparation of acenaphthol
[0051] Add 5.0g (32mmol) acenaphthene into a 100mL three-necked flask, and then add 6.5mL phosphorus oxychloride (POCl 3 ) Slowly add 13.5mL N,N-dimethylformamide (DMF) into the three-necked flask with a constant pressure funnel (the dripping is completed within 15 minutes), stir for 5 minutes and then slowly increase the temperature to 90~95℃, continue stirring 3 After hours, the reaction solution was obtained; the reaction solution was added to 270 mL of ice-water mixture, and a large amount of viscous solid appeared after stirr...
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