dodecanoyl dodecaneperoxoate

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred solution of tert-butyl 2,3-dip-tolyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (stepl) (530 mg, 1.275 mmol) in chloroform (10 ml) was added N-bromosuccinimide (272 mg, 1.531 mmol) followed by lauroyl peroxide (50.8 mg, 0.128 mmol) and the mixture was heated to reflux for 1 hour. The solvent was concentrated in vacuo. The crude product was purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane to afford the title compound which was used directly into the next step the mixture was heated to reflux for 1 hour The solvent was concentrated in vacuo The crude product was purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred solution of tert-Butyl 2,3-diphenyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (step 1)(25 g, 64.5 mmol) in carbon tetrachloride (645 ml) at RT under N2 was added NBS (13.78 g, 77 mmol) followed directly by lauroyl peroxide (0.257 g, 0.645 mmol) and the solution was heated at 60° C. for 4 h 15 mins. The mixture was filtered through filter paper and the filtrate was washed with sat. NaHCO3 (300 ml), 2 M Na2SO3 (300 ml) and sat. brine (300 ml). The solution was dried over MgSO4 and filtered, washing MgSO4 bed with DCM (100 ml). The solvent was removed in vacuo. The crude product was dissolved in diethyl ether (300 ml) and was allowed to stand at RT and placed in a fridge overnight. The resulting crystalline solid was isolated by decanting off the mother liquors. The crystals were washed with diethyl ether to afford the title compound. Further product was obtained by chromatography of the mother liquors eluting with iso-hexane/EtOAc to afford the title product; The mixture was filtered through filter paper the filtrate was washed with sat. NaHCO3 (300 ml), 2 M Na2SO3 (300 ml) and sat. brine (300 ml) The solution was dried over MgSO4 filtered washing MgSO4 bed with DCM (100 ml) The solvent was removed in vacuo The crude product was dissolved in diethyl ether (300 ml) to stand at RT The resulting crystalline solid was isolated by decanting off the mother liquors The crystals were washed with diethyl ether

Conditions: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 87.3 g of maleic anhydride and 1.46 g of dilauroyl peroxide were introduced into a 2 1 Juchheim pressurized reaction vessel, and the reaction apparatus was then flushed with nitrogen. When the apparatus was free from oxygen, 310 g of methyl vinyl ether which had been dried over solid sodium hydroxide and freshly distilled, were added. The reaction mixture was warmed to 55° C. with stirring and maintained at this temperature for 2 hours under pressure. After the mixture had cooled to 20° C., excess methyl vinyl ether was distilled off, and the reaction product was removed from the vessel. This gave 118 g (84.9 % of theory) of an MA/MVE copolymer having the following properties: loss on drying at 105° C.: 0.92 %, at 60° C. in vacuo: 0.25 %. The particle size distribution, which was measured by sieve analysis, gave the following values: the reaction apparatus was then flushed with nitrogen had been dried over solid sodium hydroxide freshly distilled were added maintained at this temperature for 2 hours under pressure After the mixture had cooled to 20° C. excess methyl vinyl ether was distilled off the reaction product was removed from the vessel loss on drying at 105° C. at 60° C. gave the following values

Conditions: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Four parts of a styrene/methacrylic acid copolymer (acid value: 250; molecular weight: 15,000) and 1 part of ELEMINOL RS-30 (trade name, product of Sanyo Chemical Industries, Ltd.) as dispersing agents were dissolved in 80 parts of dimethyl sulfoxide, and 10 parts of an isoindolinone pigment (C.I. Pigment Yellow 109) were suspended in the resultant solution in a flask at 25° C. under an air atmosphere. A 30% methanol solution of potassium hydroxide was then added dropwise little by little to dissolve the isoindolinone pigment. After the pigment solution was stirred for 3 hours, lauroyl peroxide as a polymerization initiator was added to and dissolved in the pigment solution in a proportion of 0.1 parts per 10 parts of the pigment, and the resultant solution was quickly poured into ion-exchanged water (400 parts of ion-exchanged water per 10 parts of the pigment; 0° C.) stirred by an impellor type agitating blade (800 rpm), purged with nitrogen and cooled and temperature-maintained by means of 2 system dispensers (manufactured by Musashi Engineering K.K.; needle internal diameter: 0.57 mm; delivery pressure: 4.0 kgf/cm2) to obtain an aqueous dispersion of isoindolinone-pigment-containing particles having an average particle diameter of 39.9 nm. This aqueous dispersion was transferred to a reaction vessel equipped with a mantle heater, cooling tower, stirrer and thermometer and purged with nitrogen. While continuing purging with nitrogen and stirring at 300 rpm, styrene and methacrylic acid as ethylenically unsaturated compounds were then added dropwise over 3 hours in proportions of 5.5 parts and 0.5 parts, respectively, per 10 parts of the pigment. The system was then heated to an internal temperature of 80° C. to continue the reaction for 8 hours while retaining the temperature of 80° C. After the reaction was conducted for additional 1 hour at a temperature raised to 90° C., the reaction mixture was cooled back to room temperature. (trade name, product of Sanyo Chemical Industries, Ltd.) as dispersing agents agitating blade (800 rpm) purged with nitrogen cooled temperature-maintained by means of 2 system dispensers (manufactured by Musashi Engineering K.K.; needle internal diameter: 0.57 mm; delivery pressure: 4.0 kgf/cm2)

Conditions: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 13 g (0.5 mole) of vinyl acetate, 49 g (0.5 mole) of maleic acid anhydride and 0.1 g of lauroyl peroxide were dissolved in 400 cc of benzene and heated for five hours at 70° C. The copolymer was precipitated from the viscous solution with petroleum ether (80° to 100° C.). The copolymer dissolved well in diluted caustic soda. The copolymer was precipitated from the viscous solution with petroleum ether (80° to 100° C.) The copolymer dissolved well in diluted caustic soda

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 40 parts by weight of carbon black grafted with styrene "GP-E-3" (manufactured by Ryoyu Kogyo K. K.), which contains 40% by weight of styrene monomer, 30% by weight of polystyrene and 30% by weight of grafted carbon black, 1.5 parts by weight of charge control agent of negative charging type 3-methyl-5-nitroimidazole, 4.5 parts by weight of lauroyl peroxide, 9.0 parts by weight of tolylene diisocyanate "Coronate T-100" (mfd. by Nippon Polyurethane Industry Co., Ltd.) and 0.5 part by weight of phenyl isocyanate were added to a mixture of 50 parts by weight of styrene with 35 parts by weight of 2-ethylhexyl acrylate and 0.9 part by weight of divinylbenzene to prepare a polymerizable composition. The polymerizable composition was added to 800 g of a 4 wt. % solution of calcium phosphate in an aqueous colloid previously prepared in a 2-l separable glass flask in such an amount that the concentration of the polymerizable composition became 30 % by weight based on the total of the aqueous colloid solution and the polymerizable composition. The mixture was dispersed and emulsified on a TK Homomixer mfd. by Tokushu Kika Kogyo Co., Ltd. at 10,000 rpm at 5° C. for 2 min. A four neck glass lid was placed on the flask and fitted with a reflux condenser, a thermometer, a dropping funnel having a nitrogen-inlet tube and a stainless steel stirring rod. The flask was placed in an electric mantle. A mixed solution of 24.0 g of resorcinol, 3.0 g of m-aminophenol, 2.2 g of t-butyl alcohol, 0.5 g of 1,4-diazabicyclo[2.2.2]-octane and 40 g of deionized water was prepared and added dropwise into the flask through the dropping funnel while stirring over a period of 30 min. Then the temperature was elevated to 85° C. while continuing the stirring under nitrogen and the reaction was conducted for 10 h. After cooling the reaction mixture, the dispersant was dissolved by adding 10% aqueous hydrochloric acid solution, and the mixture was filtered. The residue was washed with water, dried at 45° C. for 12 hr under a reduced pressure of 20 mmHg, and classified by means of an air classifier to give an encapsulated toner having an average particle diameter of 9 μm wherein the shell comprises a resin having thermally dissociable urethane bonds. The glass transition point of the resin in the core material of the encapsulated toner and the softening point of the encapsulated toner were 32.0° C. and 129.5° C., respectively. to prepare a polymerizable composition previously prepared in a 2-l separable glass flask in such an amount that the concentration of the polymerizable composition The mixture was dispersed fitted with a reflux condenser added dropwise into the flask through the dropping funnel was elevated to 85° C. the reaction was conducted for 10 h After cooling the reaction mixture the dispersant was dissolved the mixture was filtered The residue was washed with water dried at 45° C. for 12 hr under a reduced pressure of 20 mmHg to give an encapsulated toner were 32.0° C. and 129.5° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 40 parts by weight of carbon black grafted with styrene "GP-E-3" (manufactured by Ryoyu Kogyo K. K.), which contains 40% by weight of styrene monomer, 30% by weight of polystyrene and 30% by weight of grafted carbon black, 1.5 parts by weight of charge control agent of negative charging type 3-methyl-5-nitroimidazole, 4.5 parts by weight of lauroyl peroxide, 9.0 parts by weight of tolylene diisocyanate "Coronate T-100" (mfd. by Nippon Polyurethane Industry Co., Ltd.) and 0.5 part by weight of phenyl isocyanate were added to a mixture of 50 parts by weight of styrene with 35 parts by weight of 2-ethylhexyl acrylate and 0.9 part by weight of divinylbenzene to prepare a polymerizable composition. The polymerizable composition was added to 800 g of a 4 wt. % solution of calcium phosphate in an aqueous colloid previously prepared in a 2-l separable glass flask in such an amount that the concentration of the polymerizable composition became 30 % by weight based on the total of the aqueous colloid solution and the polymerizable composition. The mixture was dispersed and emulsified on a TK Homomixer mfd. by Tokushu Kika Kogyo Co., Ltd. at 10,000 rpm at 5° C. for 2 min. A four neck glass lid was placed on the flask and fitted with a reflux condenser, a thermometer, a dropping funnel having a nitrogen-inlet tube and a stainless steel stirring rod. The flask was placed in an electric mantle. A mixed solution of 24.0 g of resorcinol, 3.0 g of m-aminophenol, 2.2 g of t-butyl alcohol, 0.5 g of 1,4-diazabicyclo[2.2.2]-octane and 40 g of deionized water was prepared and added dropwise into the flask through the dropping funnel while stirring over a period of 30 min. Then the temperature was elevated to 85° C. while continuing the stirring under nitrogen and the reaction was conducted for 10 h. After cooling the reaction mixture, the dispersant was dissolved by adding 10% aqueous hydrochloric acid solution, and the mixture was filtered. The residue was washed with water, dried at 45° C. for 12 hr under a reduced pressure of 20 mmHg, and classified by means of an air classifier to give an encapsulated toner having an average particle diameter of 9 μm wherein the shell comprises a resin having thermally dissociable urethane bonds. The glass transition point of the resin in the core material of the encapsulated toner and the softening point of the encapsulated toner were 32.0° C. and 129.5° C., respectively. to prepare a polymerizable composition previously prepared in a 2-l separable glass flask in such an amount that the concentration of the polymerizable composition The mixture was dispersed fitted with a reflux condenser added dropwise into the flask through the dropping funnel was elevated to 85° C. the reaction was conducted for 10 h After cooling the reaction mixture the dispersant was dissolved the mixture was filtered The residue was washed with water dried at 45° C. for 12 hr under a reduced pressure of 20 mmHg to give an encapsulated toner were 32.0° C. and 129.5° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred solution of tert-butyl 2,3-dip-tolyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (stepl) (530 mg, 1.275 mmol) in chloroform (10 ml) was added N-bromosuccinimide (272 mg, 1.531 mmol) followed by lauroyl peroxide (50.8 mg, 0.128 mmol) and the mixture was heated to reflux for 1 hour. The solvent was concentrated in vacuo. The crude product was purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane to afford the title compound which was used directly into the next step the mixture was heated to reflux for 1 hour The solvent was concentrated in vacuo The crude product was purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred solution of tert-butyl 2,3-dip-tolyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (stepl) (530 mg, 1.275 mmol) in chloroform (10 ml) was added N-bromosuccinimide (272 mg, 1.531 mmol) followed by lauroyl peroxide (50.8 mg, 0.128 mmol) and the mixture was heated to reflux for 1 hour. The solvent was concentrated in vacuo. The crude product was purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane to afford the title compound which was used directly into the next step the mixture was heated to reflux for 1 hour The solvent was concentrated in vacuo The crude product was purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred solution of tert-Butyl 2,3-diphenyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (step 1)(25 g, 64.5 mmol) in carbon tetrachloride (645 ml) at RT under N2 was added NBS (13.78 g, 77 mmol) followed directly by lauroyl peroxide (0.257 g, 0.645 mmol) and the solution was heated at 60° C. for 4 h 15 mins. The mixture was filtered through filter paper and the filtrate was washed with sat. NaHCO3 (300 ml), 2 M Na2SO3 (300 ml) and sat. brine (300 ml). The solution was dried over MgSO4 and filtered, washing MgSO4 bed with DCM (100 ml). The solvent was removed in vacuo. The crude product was dissolved in diethyl ether (300 ml) and was allowed to stand at RT and placed in a fridge overnight. The resulting crystalline solid was isolated by decanting off the mother liquors. The crystals were washed with diethyl ether to afford the title compound. Further product was obtained by chromatography of the mother liquors eluting with iso-hexane/EtOAc to afford the title product; The mixture was filtered through filter paper the filtrate was washed with sat. NaHCO3 (300 ml), 2 M Na2SO3 (300 ml) and sat. brine (300 ml) The solution was dried over MgSO4 filtered washing MgSO4 bed with DCM (100 ml) The solvent was removed in vacuo The crude product was dissolved in diethyl ether (300 ml) to stand at RT The resulting crystalline solid was isolated by decanting off the mother liquors The crystals were washed with diethyl ether

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred solution of tert-Butyl 2,3-diphenyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (step 1)(25 g, 64.5 mmol) in carbon tetrachloride (645 ml) at RT under N2 was added NBS (13.78 g, 77 mmol) followed directly by lauroyl peroxide (0.257 g, 0.645 mmol) and the solution was heated at 60° C. for 4 h 15 mins. The mixture was filtered through filter paper and the filtrate was washed with sat. NaHCO3 (300 ml), 2 M Na2SO3 (300 ml) and sat. brine (300 ml). The solution was dried over MgSO4 and filtered, washing MgSO4 bed with DCM (100 ml). The solvent was removed in vacuo. The crude product was dissolved in diethyl ether (300 ml) and was allowed to stand at RT and placed in a fridge overnight. The resulting crystalline solid was isolated by decanting off the mother liquors. The crystals were washed with diethyl ether to afford the title compound. Further product was obtained by chromatography of the mother liquors eluting with iso-hexane/EtOAc to afford the title product; The mixture was filtered through filter paper the filtrate was washed with sat. NaHCO3 (300 ml), 2 M Na2SO3 (300 ml) and sat. brine (300 ml) The solution was dried over MgSO4 filtered washing MgSO4 bed with DCM (100 ml) The solvent was removed in vacuo The crude product was dissolved in diethyl ether (300 ml) to stand at RT The resulting crystalline solid was isolated by decanting off the mother liquors The crystals were washed with diethyl ether