Benzindole salt material, its nonlinear optical crystal, preparation method and use
A benzo and indole technology, which is applied in the field of nonlinear optics, can solve the problems that the molecular arrangement is not optimized, does not have second-order nonlinearity, and the crystal growth conditions are harsh. Linear response, easy-to-process effects
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Embodiment 1
[0052] (E)-2-(4-(Dimethylamino)styryl)-1,1,3-trimethyl-1H-benzo[e]indole-3-iodide salt
[0053] In general formula (1), when R is a benzene ring, X is I -, the benzindole salt material is (E)-2-(4-(dimethylamino)styryl)-1,1,3-trimethyl-1H-benzo[e]indole -3-Iodine salt (molecular formula C 25 h 25 N 2 1, molecular weight 482), its preparation method is as shown in following reaction scheme 1:
[0054]
[0055] Wherein 1 is solvent methanol, 2 is solvent ethanol, catalyst piperidine
[0056] This method mainly includes the following two parts I and II:
[0057] Synthesis of I.1,1,2,3-tetramethyl-1H-benzo[e]indole-3-iodide salt:
[0058] Add 20 mL of anhydrous methanol, 17.6 mmol (2.5 g) of methyl iodide and 17.6 mmol (3.7 g) of 1,1,2-trimethyl-1H-benzo[e]indole raw materials into a round bottom flask, and heat to reflux ( Preferably 6h), cooled to room temperature, filtered off the solid, and dried in vacuo to finally obtain light blue 1,1,2,3-tetramethyl-1H-benzo[e]in...
Embodiment 11
[0076] (E)-2-(4-(Dimethylamino)styryl)-1,1,3-trimethyl-1H-benzo[e]indole-3-iodo When the salt crystal is observed under a polarizing microscope, when the crystal is rotated along the incident direction of the light, when the direction of the polarizer is neither parallel nor perpendicular to the optical axis, the light can pass through and the crystal is transparent; but when the polarizer is parallel to the optical axis, the crystal darken. For polycrystals, light and dark parts exist simultaneously during rotation. Through this method of rotating and observing the light and shade of the crystal, we can judge whether it is single crystal or polycrystalline. attached figure 2 And attached image 3 It can be judged that the crystal grown in the present invention is a single crystal.
[0077] X-ray crystal diffraction results show that the crystal of the present invention belongs to the monoclinic crystal system, and the space group is P2 1 , formula C 25 h 25 N 2 I, FM...
Embodiment 12
[0082] (E)-2-(4-(dimethylamino)styryl)-1,1,3-trimethyl-1H-benzo[e] obtained in the above growth in dimethyl sulfoxide solvent The indole-3-iodide salt crystal is observed under a polarizing microscope. When the crystal is rotated along the incident direction of the light, when the direction of the polarizer is neither parallel nor perpendicular to the optical axis, the light can pass through and the crystal is transparent; but when the polarizer When parallel to the optical axis, the crystal becomes darker. For polycrystals, light and dark parts exist simultaneously during rotation. Through this method of rotating and observing the light and shade of the crystal, we can judge whether it is single crystal or polycrystalline. attached Figure 6 And attached Figure 7It can be judged that the crystal grown in the present invention is a single crystal.
[0083] X-ray crystal diffraction results show that the crystal of the present invention belongs to the monoclinic crystal sy...
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