Photochromic compound and its preparation method and application
A compound and selected technology, applied in chemical instruments and methods, color-changing fluorescent materials, organic chemistry, etc., can solve problems such as photochemical side reactions, limit the application of r-spiropyran, and affect the number of reversible conversion cycles
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Embodiment 1
[0033] (1) Add 2.5g (62.4mmol) NaOH and 100ml water into a four-neck flask, stir to dissolve at 60°C, then add 10g (62.4mmol) 2,7-dihydroxynaphthalene, stir at 60°C for 30min, and wait for dissolution After adding 5.2g (74.80mmol) NaNO 2 , stirred for 20 min, cooled to 0° C. in an ice-salt bath, slowly added dropwise a mixture of 8 mL of concentrated sulfuric acid and 15 mL of water at this temperature, and continued to react for 3 h after the addition was complete. After the reaction was completed, 11.33 g of a reddish-brown solid was obtained after suction filtration, and the yield was 96.2%. Elemental Analysis, C 10 h 7 o 3 N: found value (theoretical value) / %: C 63.49 (63.52); H 3.71 (3.70); H 7.43 (7.41).
[0034]
[0035] (2) Under a nitrogen atmosphere, add 9.45g (0.05mol) of 1-nitroso-2,7-dihydroxynaphthalene and 600mL of anhydrous methanol to a 1000mL four-neck flask, reflux and stir for 1h, and then add 2 times the equivalent of indole Dole, stirred at reflux...
Embodiment 2
[0043] Using the same method as in Example 1, replacing indole with pyrrole and p-phenylbenzoyl chloride with p-naphthylbenzoyl chloride, 1,3-dimethyl-6'-pyrrolyl-9 '-[p-naphthylbenzoyloxy]-1,3 dihydrospiro[benzimidazole-2,3'-naphtho[2,1-b][1,4]oxazine. The yield was 53.1%.
[0044] The photochromic substance is configured into 1×10 with chloroform -5 mol / L dilute solution, and then irradiated with 365nm ultraviolet light, it can be observed that the color of its chloroform solution changes from colorless to blue-green, and at the same time, it can be observed with an ultraviolet spectrophotometer (U.S. after 623nm -1 The maximum absorption peak appears.
Embodiment 3
[0046] Using the same method as in Example 1, replacing indole with imidazole, and p-phenylbenzoyl chloride with p-anthracenylbenzoyl chloride, 1,3-dimethyl-6'-imidazolyl-9 '-[p-Anthracenylbenzoyloxy]-1,3 dihydrospiro[benzimidazole-2,3'-naphtho[2,1-b][1,4]oxazine. The yield was 51.8%.
[0047] The photochromic substance is configured into 1×10 with chloroform -5 mol / L dilute solution, and then irradiated with 365nm ultraviolet light, it can be observed that the color of its chloroform solution changes from colorless to pink purple, and at the same time, it can be observed with a UV spectrophotometer (Varian UV1101, USA). after 620nm -1 The maximum absorption peak appears. The above-mentioned embodiments only illustrate the principles and effects of the present invention, but are not intended to limit the present invention. Anyone skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Th...
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