Piperazino photoinitiation sensitiser
A compound and group technology, applied in the field of piperazine sensitizers, can solve problems such as unfavorable hydrogen abstraction and Michler's ketone not being particularly effective
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Embodiment 1
[0071] Preparation of 4,4'-dipiperazinylbenzophenone
[0072]
[0073] 5.0 g of 4,4'-difluorobenzophenone (0.0229 mol), 3.94 g of piperazine (0.0458 mol), 6.60 g of potassium carbonate powder (0.0478 mol) and 50 ml of anhydrous DMSO (dimethyl sulfone) were mixed in a three-necked flask equipped with stirrer, nitrogen inlet, condenser, calcium chloride drying tube / nitrogen outlet and temperature sensor. The mixture was heated to reflux under a constant flow of nitrogen for 12 hours (-190 °C). The mixture was then cooled to room temperature and filtered to remove inorganics. The reaction flask was rinsed with an additional 75ml DMSO. The DMSO solution was then added to 100 g of water. The resulting mixture was extracted with dichloromethane (3x75ml). The dichloromethane layers were combined and washed with 100 ml of saturated sodium chloride solution. The dichloromethane layer was then dried over anhydrous magnesium sulfate. Magnesium sulfate was removed by filtration, ...
Embodiment 2
[0079]
[0080]2.84 g of propoxylated neopentyl glycol diacrylate (PNPGDA, molecular weight 328) (0.00866 mol), 2.00 g of the product of Example 1 (4,4'-dipiperazinylbenzophenone) (0.00571 mol), toluene 30ml and 0.115g of 1,8-diazabicyclo(5.4.0)undec-7-ene (DBU) (catalyst) in a two-neck round bottom equipped with stirrer, condenser and temperature sensor Mix in the flask. The mixture was heated to reflux for a total of 10 hours (over 2 days). The mixture was then cooled and filtered to remove unreacted 4,4'-dipiperazinylbenzophenone, then the solvent was removed on a rotary evaporator to give the product.
[0081] The yield of the product was 4.95 g as a viscous slightly yellow liquid.
[0082] The product was analyzed by GPC.
[0083] GPC: Mn 5167, Mw 11664.
Embodiment 3
[0085]
[0086] 2.60g tripropylene glycol diacrylate (TPGDA, molecular weight 300) (0.00866 mol), the product (4,4'-dipiperazinyl benzophenone) (0.00433 mol) of embodiment 1 of 1.515g, toluene 30ml and 0.115 g of 1,8-diazabicyclo(5.4.0)undec-7-ene (DBU) (catalyst) were mixed in a two necked round bottom flask equipped with stirrer, condenser and temperature sensor. The mixture was heated to reflux for a total of 10 hours (over 2 days). The mixture was then cooled and filtered to remove unreacted 4,4'-dipiperazinylbenzophenone, then the solvent was removed on a rotary evaporator to give the product.
[0087] Product yield 3.77 g (91.6%) as a viscous yellowish liquid.
[0088] The product was analyzed by GPC.
[0089] GPC: Mn 3165, Mw 3885.
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