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Example 3
37 parts of ethylene glycol monobutyl ether was placed in a reactor equipped with a thermometer, a thermostat, a stirrer, a reflux condenser, and a dropping funnel; and heated with stirring to maintain the reaction mixture at 110° C. A mixture of 10 parts of styrene, 35 parts of methyl methacrylate, 20 parts of 2-ethylhexyl methacrylate, 5 parts of N,N-dimethylaminoethyl methacrylate, 10 parts of 2-hydroxyethyl methacrylate, 20 parts of methoxy polyethylene glycol monomethacrylate (molecular weight: about 2080), 1 part of azobisisobutyronitrile, and 5 parts of isobutyl alcohol was added dropwise thereto over 3 hours. After the completion of dropwise addition, the mixture was aged at 110° C. for 30 minutes. Subsequently, an additional catalyst mixture of 20 parts of ethylene glycol monobutyl ether and 0.5 parts of azobisisobutyronitrile was added dropwise over 1 hour. After aging at 110° C. for 1 hour, the mixture was cooled, thereby obtaining an acrylic resin (R-3) solution with a solids content of 50%. The obtained resin had a weight average molecular weight of 20000.
Example 3
Eudragit® E PO (EPO) is a cationic copolymer based on dimethylaminoethyl methacrylate, butyl methacrylate, and methyl methacrylate. Technical literature indicates that this polymer is soluble in acid, up to pH 5; above pH 5 it swells rather than dissolves. Dry granulations containing 5% alprazolam in EPO polymer were prepared and size fractions collected at −16 mesh and +20 mesh (16/20) and at −20 mesh and +30 mesh (20/30). Dissolution on the granulation size fractions were performed at both low pH (pH 1.5) where EPO is soluble and at high pH (pH 6) were EPO is less soluble. The results are shown in
Example 2
In a four-necked flask of 1 liter equipped with a well-dried stirring blade and a thermometer, 416 g (3.20 mol) of HEMA, 0.75 g of DBTDL (0.1% by mass with respect to the total mass of HEMA and TMHDI), and 0.38 g of MEHQ (0.05% by mass of the total mass of HEMA and TMHDI) were added and stirred until the mixture was homogeneous, and then the temperature was raised to 60° C. Subsequently, 337 g of TMHDI (1.60 mol) was added dropwise over 1 hour. As the internal temperature rose due to the reaction heat during the drop, the drop rate was controlled so that the temperature was below 80° C. After completion of the dropping of the total amount, the reaction was carried out for 10 hours while keeping the temperature at 80° C. At this time, the proceedings of reaction were tracked by HPLC analysis to confirm the endpoint of the reaction. The product was discharged from the reactor to obtain 720 g of a bifunctional urethane methacrylate (UDMA). The viscosity at 25° C. was 8,200 mPa·s.