Oxime ester photoinitiator and preparation method thereof
A technology of photoinitiator and oxime ester, which is applied in the field of photoinitiator and its preparation of unsaturated resin photoinitiated polymerization, can solve the problems of low yield, unsuitable for industrial production, environmentally harmful waste, etc., and achieve short reaction time , low production cost, good safety effect
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Embodiment 1
[0030] a. Intermediate one preparation of
[0031] Add 111.8g of diphenyl sulfide (0.6mol), 1mol of zirconium catalyst and 600ml of dichloromethane into a four-necked flask equipped with an electric stirrer and a thermometer, pass through nitrogen protection, and reduce the temperature of the reaction solution to -5~ 0°C, and then dropwise added a mixed solution of 110.0g 4-chlorobutyryl chloride (0.78mol) and 150g of dichloromethane, and after the dropwise addition was completed, the temperature was raised to 15°C and stirring was continued for 2 hours. After the reaction was completed, the reaction solution was poured into 2000ml of 1mol / L dilute sulfuric acid, and the lower organic phase was separated. The aqueous phase was extracted with 300 ml of dichloromethane. The organic phases were combined, washed once with 500ml of saturated sodium bicarbonate solution, and then washed three times with 500ml of water until neutral, added 200g of anhydrous magnesium sulfate for d...
Embodiment 2
[0039] The preparation of a.1-diphenylsulfide group-4-chlorobutanone
[0040] Add 111.8 g of diphenyl sulfide (0.6 mol), 2 mol of zirconium catalyst and 500 ml of chloroform into a four-necked flask equipped with an electric stirrer and a thermometer, pass through nitrogen protection, and lower the temperature of the reaction solution to 0-5°C. Then, a mixed solution of 126.9 g of 4-chlorobutyryl chloride (0.9 mol) and 200 g of chloroform was added dropwise, and after the dropwise addition, the temperature was raised to 15° C. and stirring was continued for 2 hours. After the reaction was completed, the reaction solution was poured into 2000ml of 2mol / L dilute hydrochloric acid, and the lower organic phase was separated. The aqueous phase was extracted with 300 ml of chloroform. Combine the organic phases, wash once with 500ml of saturated sodium bicarbonate solution, then wash three times with 500ml of water until neutral, add 200g of anhydrous magnesium sulfate to dry, and ...
Embodiment 3
[0048] a. Intermediate one preparation of
[0049] Add 100.5g of N-ethylcarbazole (0.51mol) and 300ml of dichloromethane into a four-necked flask equipped with an electric stirrer and a thermometer, lower the temperature of the reaction solution to -10~0°C, add 1mol of zirconium catalyst, Then a mixed solution of 102.0 g of o-toluyl chloride (0.66 mol) and 100 ml of dichloromethane was added dropwise, and after the dropwise addition was completed, the mixture was incubated and stirred for 1 hour. Then, a mixed solution of 74.5 g of chloroacetyl chloride (0.66 mol) and 50 ml of dichloromethane was added, and the stirring reaction was continued for 30 minutes. After the reaction is complete, pour the reaction solution into 1500ml of 1mol / L dilute hydrochloric acid, stir for 1 hour, separate the liquids, and wash with water until neutral. The solvent was distilled off under reduced pressure, 1000ml of ethanol was added to make a slurry, suction filtered and dried to obtain 165...
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