Assisted initiator amine-containing polymerizable thioxanthone carbazole visible light photoinitiator and preparation method thereof
A thioxanthone carbazole-based, visible light technology, applied in organic chemistry and other directions, can solve the problems of easy migration of fragments, odor toxicity, poor compatibility, etc.
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Embodiment 1
[0049] The product of the present invention 3-(diethylamino)-2-(13-oxothiochromeno[2,3-B]carbazol-7-(13H)-yl)propyl methacrylate, which The structural formula is:
[0050]
[0051] Preparation of product 3-(diethylamino)-2-(13-oxothiochromeno[2,3-B]carbazol-7-(13H)-yl)propyl methacrylate of the present invention method, the detailed steps are as follows:
[0052] a. Put 29.24g (0.4mol) of diethylamine into a 100ml reaction flask, start stirring, heat to 56°C, slowly add 28.40g (0.2mol) of glycidyl methacrylate (GMA) into the reaction flask, and react 2h; warming up to 80°C, reacting for 3h; after the reaction, the resulting reactant was distilled to remove residual diethylamine to obtain 42.80g 3-(diethylamino)-2-hydroxypropyl methacrylate ( GMA-DEA) (see the attached infrared spectrum figure 1 );
[0053] b. Add 4.30g (0.02mol) of GMA-DEA and 0.79g (0.01mol) of pyridine into a 100ml reaction flask containing 30ml (44.50g) of chloroform at 1 to 3°C, and then dropwise a...
Embodiment 2
[0057] Embodiment 2: basically the same as Embodiment 1, the difference is:
[0058] Preparation of product 3-(diethylamino)-2-(13-oxothiochromeno[2,3-B]carbazol-7-(13H)-yl)propyl methacrylate of the present invention method, the detailed steps are as follows:
[0059] a. Put 29.24g (0.4mol) of diethylamine into a 100ml reaction bottle, start stirring, heat to 40°C, slowly add 28.40g (0.2mol) of GMA into the reaction bottle, react for 1h; raise the temperature to 70°C for 4h ; After the reaction finished, the gained reactant was distilled to remove remaining diethylamine to obtain 42.08g GMA-DEA;
[0060] b. Add 4.30g (0.02mol) GMA-DEA into a 100ml reaction flask containing 40ml (59.20g) chloroform at 1-3°C, then add 5.40g (0.02mol) PBr dropwise 3 and a mixed solution of 10ml (14.80g) chloroform, reacted at 1-3°C for 1h; raised the temperature to 70°C for 4h;
[0061]After the reaction finished, the gained reactant was cooled to 20°C, added in 15ml of distilled water, then ...
Embodiment 3
[0064] Embodiment 3: basically the same as Embodiment 1, the difference is:
[0065] Preparation of product 3-(diethylamino)-2-(13-oxothiochromeno[2,3-B]carbazol-7-(13H)-yl)propyl methacrylate of the present invention method, the detailed steps are as follows:
[0066] a. Put 14.63g (0.2mol) of diethylamine into a 100ml reaction flask, start stirring, and heat to 60°C; slowly add 28.40g (0.2mol) of GMA into the reaction flask at this temperature, and react for 4 hours; heat up to Reaction at 70°C for 3 hours; after the reaction, the obtained reactant was distilled to remove residual diethylamine to obtain 38.95 g of GMA-DEA;
[0067] b. Add 4.30g (0.02mol) GMA-DEA and 1.58g (0.02mol) pyridine into a 100ml reaction flask containing 50ml (74.00g) chloroform at 1-3°C, then add 16.20g (0.06 mol)PBr 3 and a mixed solution of 15ml (22.20g) of chloroform, reacted at 1-3°C for 2h; raised the temperature to 40°C for 5h;
[0068] After the reaction was finished, the gained reactant ...
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