A piezochromic fluorescent molecule and its preparation method and application
A fluorescent molecule, piezochromic technology, applied in the direction of color-changing fluorescent materials, chemical instruments and methods, imino compound preparation, etc. Effect
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[0049] The present invention provides a method for preparing piezochromic fluorescent molecules described in the above technical solution, comprising the following steps:
[0050] (1) Mix 1,1,3,3-tetramethoxypropane, arylamine and an organic solvent to obtain a mixed solution; the arylamine is aniline or p-bromoaniline;
[0051] (2) Cool down the mixed solution obtained in the step (1) to -5-5°C, add acid solution dropwise, carry out hydrolysis and nucleophilic addition reaction, and obtain piezochromic fluorescent molecules.
[0052] The invention mixes 1,1,3,3-tetramethoxypropane, arylamine and organic solvent to obtain a mixed solution. In the present invention, the arylamine is aniline or p-bromoaniline. In the present invention, when the arylamine is aniline and p-bromoaniline, the obtained products correspond to compounds in which R in formula I is R1 and R3, respectively. In the present invention, there is no special limitation on the ratio of the 1,1,3,3-tetramethoxypr...
Embodiment 1
[0067] The synthesis of N-((1E)-3-(phenylimino) prop-1-en-1-yl) aniline hydrochloride (N1), the reaction equation is as follows:
[0068]
[0069] Add 3.284g (0.02mol, 1eq.) of 1,1,3,3-tetramethoxypropane, 3.720g (0.04mol, 2eq.) of aniline and 50ml of absolute ethanol into a 100mL two-necked flask, stir to dissolve completely Cool the solution to 0°C, slowly add 4ml of concentrated hydrochloric acid dropwise within 15 minutes with a constant pressure dropping funnel, continue to stir at room temperature for 1-2 hours after the dropwise addition, a yellow solid precipitates, filter with suction, wash the filter cake with water and ethanol respectively After 3 times of vacuum drying, an orange-yellow product was obtained with a yield of 55%.
[0070] Test results: 1H NMRδ12.70(s, 2H), 8.925(d, J=6.0Hz, 2H), 7.43-7.50(m, 8H), 7.25(t, J=4.0Hz, 2H), 6.51(t, J=12Hz,1H),
[0071] Elemental Analysis: Grouped C 15 h 15 ClN 2 .
[0072] Theoretical calculations: C, 69.63; H, 5....
Embodiment 2
[0087] The synthesis of 4-bromo-N-((1E)-3-((4-bromophenyl)imino)prop-1-en-1-yl)aniline hydrochloride (N3) is as follows:
[0088]
[0089] The process is the same as in Example 1, except that the reactant aniline is replaced by p-bromoaniline, and the yellow product is obtained by vacuum drying with a yield of 83%.
[0090] Test results: 1H NMRδ12.74(s, 2H), 8.815(d, J=6.0Hz, 2H), 7.70(d, J=4.0Hz, 4H), 7.37(d, J=4.0Hz, 4H), 6.51 (t, J = 12Hz, 1H).
[0091] Elemental analysis: Molecular formula C 15 h 13 Br 2 ClN 2 .
[0092] Calculated theoretically: C, 43.25; H, 3.15; N, 6.73.
[0093] Actual measured values: C, 43.29; H, 3.13; N, 6.70.
[0094] High resolution mass spectrometry: Calculated value of ion peaks [M-Cl - ]: 380.9440.
[0095] Measured value: 380.9436.
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