Dendritic macromolecular photoinitiator with low biotoxicity as well as preparation and application of dendritic macromolecular photoinitiator
A low biological toxicity, photoinitiator technology, applied in the direction of organic chemistry, can solve the problem of decreased solubility and achieve the effect of reduced mobility and low biological toxicity
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Embodiment 1
[0044] Embodiment 1: Synthesize according to the following route
[0045]
[0046] (a): A magnetic stirrer was placed in a 100mL three-neck flask equipped with a constant pressure dropping funnel and a condenser, and 1.98g (1eq) of 3-methyldibenzothiophene and 200ml of anhydrous dibenzothiophene were added sequentially in an ice bath. Chloromethane (solvent), 3.62g (2.5eq) aluminum trichloride (catalyst), after stirring evenly, slowly add 1.83g (1.5eq) methyl oxalyl chloride (acylating reagent), keep the system temperature below 10°C, After the dropwise addition, return to room temperature and react for about 4 hours, and track through a thin-layer silica gel plate during the reaction. After the reaction was complete, the mixture was poured into ice water, hydrochloric acid was added dropwise for hydrolysis, extracted with dichloromethane, the organic layer was washed with saturated sodium chloride solution until neutral, dried with anhydrous sodium sulfate, and the organic...
Embodiment 2
[0049] Embodiment 2: Synthesize according to the following route
[0050]
[0051] The synthesis method of compound (I)-b is the same as Example 1, and will not be described in detail here.
[0052] (c): with 1.81g (1eq) compound (I)-b, 0.48g (0.2eq) end is the branched polyamidoamine of 4 hydroxyls and 1.22g (2eq) K 2 CO 3 Add there-necked flask, 5ml DMF is used as solvent, heat to solvent reflux, react about 4h, after cooling, filter off inorganic salt, solution is dripped in anhydrous ether, product is separated out, after filtering, dry to constant weight, obtain target product (I )-40.72g, yield 62.1%.
Embodiment 3
[0053] Embodiment 3: Synthesize according to the following route
[0054]
[0055] The synthesis method of compound (I)-b is the same as Example 1, and will not be described in detail here.
[0056] (c): with 3.62g (1eq) compound (I)-b, 1.37g (0.1eq) end is the branched polyamide amine of 8 amino groups and 2.76g (2eq) K 2 CO 3 Add three-necked flask, 15ml DMF as solvent, heat to solvent reflux, react for about 4h, after cooling, filter off inorganic salt, solution is added dropwise in a large amount of anhydrous diethyl ether, product precipitates, after filtering, dry to constant weight, obtain target product ( I) - 73.02 g, yield 83.4%.
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