Thiophene derivative for DNA detection and preparation method thereof
A technology of thiophene derivatives and thiophene acetic acid, which is applied in the fields of biochemical equipment and methods, determination/inspection of microorganisms, organic chemistry, etc., can solve the problems of less reports of complex formation and interference, etc.
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Embodiment 1
[0023] Weigh 3.34ml (50mmol) of ethylenediamine and 1ml of triethylamine and dissolve it in 30ml of chloroform, lower the temperature to 0°C, weigh di-tert-butyl dicarbonate (1.09g, 5mmol) and dissolve it in 20ml of chloroform and slowly add it dropwise into the above solution, stirred and reacted for 3 hours, then the reaction solution gradually rose to room temperature (about 25° C.), and continued to react for 10 hours. After the reaction, insoluble matter was removed by filtration, unreacted ethylenediamine was removed by a rotary evaporator, and concentrated to obtain a light yellow oily liquid which was compound 1 (0.71 g, 89%). 1 H-NMR: (400MHZ, CDCL 3 , ppm): δ1.45(s, 9H), 1.74(s, 2H), 2.78(t, 2H), 3.17(q, 2H), 5.12(broad s, 1H).
Embodiment 2
[0025] Weigh 10ml (99.5mmol) of 1,4-butanediamine and dissolve it in 70ml of dichloromethane, lower the temperature to 0°C, weigh di-tert-butyl dicarbonate (7.24g 33.2mmol) and dissolve it in 20ml of chloroform and slowly Add it dropwise to the above solution, stir and react for 3 hours, then the reaction solution gradually rises to room temperature (about 25° C.), and continue to react for 10 hours. After the reaction was completed, 70 ml of chloroform was added to the mixed solution for dilution, washed with 5% sodium carbonate solution, dried over anhydrous magnesium sulfate, and excess solvent was removed with a rotary evaporator. The residue was dissolved in 10 ml of 1M aqueous hydrochloric acid and washed twice with ether. The resulting aqueous layer was made basic (pH = 10) with 2M aqueous sodium hydride solution, and then extracted with ethyl acetate. The extract was dried with anhydrous magnesium sulfate, and the excess solvent was removed to obtain compound 2 withou...
Embodiment 3
[0027] Compound 3 can be prepared by using 1,6-hexanediamine instead of 1,4-butanediamine in Example 2, and the synthesis method is the same as that of Example 2. 1 H-NMR: (400MHZ, CDCL 3 , ppm): δ1.55-1.27 (m, 17H), 2.67 (t, 2H), 3.11 (q, 2H), 4.90 (broad s, 1H).
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