1,3-Bis(3-aminopropyl)tetramethyldisiloxane[Monomerforsiliconmodifiedpolyamides]

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 5 liters four-necked flask equipped with a stirrer, a thermometer, a gas-inlet tube, and a condenser were placed 1000 g (4.0 moles) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetra-methyldisiloxane having a gas chromatography purity of 98.4%, and 2,600 g of isopropanol. 360 g (9.9 moles) of hydrogen chloride gas was bubbled into the solution while stirring the mixture at room temperature. Recrystallization was conducted to obtain 1,250 g (yield: 97%) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which was an acid addition salt. In a 5 liters four-necked flask equipped with a stirrer Recrystallization

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 500 ml four-necked flask equipped with a stirrer, a thermometer, a condenser, and a dropping funnel was placed 24.9 g (0.1 mole) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane having a gas chromatography purity of 98.4%. 31.3 g (0.3 mole) of concentrated hydrochloric acid was dropwise added to the flask, and the resulting mixture was stirred at room temperature for 30 minutes. 300 g of isopropanol was added to the solution. The resulting mixture was heated under reduced pressure, and isopropanol was distilled off while conducting azeotropic distillation, to obtain a concentrated and dried product. The concentrated and dried product thus obtained was recrystallized from isopropanol to obtain 28.9 g (yield: 90%) of 1,3-bis(3-amino-propyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which is an acid addition salt. In a 500 ml four-necked flask equipped with a stirrer was distilled off distillation to obtain a concentrated The concentrated dried product thus obtained was recrystallized from isopropanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 5 liters four-necked flask equipped with a stirrer, a thermometer, a gas-inlet tube, and a condenser were placed 1000 g (4.0 moles) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetra-methyldisiloxane having a gas chromatography purity of 98.4%, and 2,600 g of isopropanol. 360 g (9.9 moles) of hydrogen chloride gas was bubbled into the solution while stirring the mixture at room temperature. Recrystallization was conducted to obtain 1,250 g (yield: 97%) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which was an acid addition salt. In a 5 liters four-necked flask equipped with a stirrer Recrystallization

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 500 ml four-necked flask equipped with a stirrer, a thermometer, a condenser, and a dropping funnel was placed 24.9 g (0.1 mole) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane having a gas chromatography purity of 98.4%. 31.3 g (0.3 mole) of concentrated hydrochloric acid was dropwise added to the flask, and the resulting mixture was stirred at room temperature for 30 minutes. 300 g of isopropanol was added to the solution. The resulting mixture was heated under reduced pressure, and isopropanol was distilled off while conducting azeotropic distillation, to obtain a concentrated and dried product. The concentrated and dried product thus obtained was recrystallized from isopropanol to obtain 28.9 g (yield: 90%) of 1,3-bis(3-amino-propyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which is an acid addition salt. In a 500 ml four-necked flask equipped with a stirrer was distilled off distillation to obtain a concentrated The concentrated dried product thus obtained was recrystallized from isopropanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 500 ml four-necked flask equipped with a stirrer, a thermometer, a condenser, and a dropping funnel was placed 24.9 g (0.1 mole) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane having a gas chromatography purity of 98.4%. 31.3 g (0.3 mole) of concentrated hydrochloric acid was dropwise added to the flask, and the resulting mixture was stirred at room temperature for 30 minutes. 300 g of isopropanol was added to the solution. The resulting mixture was heated under reduced pressure, and isopropanol was distilled off while conducting azeotropic distillation, to obtain a concentrated and dried product. The concentrated and dried product thus obtained was recrystallized from isopropanol to obtain 28.9 g (yield: 90%) of 1,3-bis(3-amino-propyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which is an acid addition salt. In a 500 ml four-necked flask equipped with a stirrer was distilled off distillation to obtain a concentrated The concentrated dried product thus obtained was recrystallized from isopropanol

反応条件: temp:180.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 300 ml flask fitted with a thermometer, a stirrer, a condenser, and a nitrogen inlet tube was charged with 2.71 g (0.045 mols) of 1,12-diaminododecane, 5.77 g (0.01 mols) of a polyetherdiamine (ED2000 (a product name), manufactured by BASF Corporation, molecular weight: 1,923), 3.35 g (0.045 mols) of 1,3-bis(3-aminopropyl)tetramethyldisiloxane (LP-7100 (a product name), manufactured by Shin-Etsu Chemical Co., Ltd.), 15.62 g (0.1 mols) of 4,4′-(4,4′-isopropylidenediphenoxy)bis(phthalic anhydride) that had been purified in advance by recrystallization from acetic anhydride (and exhibited a difference between the endothermic start temperature and the endothermic peak temperature as determined by DSC of 2.5° C.), and 113 g of N-methyl-2-pyrrolidone, and the resulting reaction liquid was then heated to 180° C. under constant stirring while nitrogen gas was blown through the system, thereby allowing the reaction to progress. The water generated within the reaction liquid was then removed, yielding a solution of a polyimide resin (PI-C). Measurement of the polyimide resin by GPC revealed polystyrene equivalent values of Mn=22,600 and Mw=121,400. A 300 ml flask fitted with a thermometer, a stirrer, a condenser, and a nitrogen inlet tube as determined by DSC of 2.5° C. the resulting reaction liquid the reaction was then removed

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In accordance with the procedure of Preparation Example 1, a polyimide resin solution was obtained using 288 grams (0.98 mol) of 3,3,4,4-biphenyltetracarboxylic dianhydride as a tetracarboxylic dianhydride component, 74.6 grams (0.3 mol) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and 287.4 grams (0.7 mol) of 2,2-bis[4-(4-aminophenoxy)-phenyl]propane as diamine components, 6 grams (0.04 mol) of phthalic anhydride as a molecular weight modifier, and 2,600 grams of NMP as a solvent. The solution was poured into 5 liters of methanol whereupon a precipitate settled out. Vacuum drying yielded 615 grams of the end polyimide resin. Vacuum drying

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 250 ml three-neck round-bottom flask equipped with a magnetic stirrer, argon inlet, and condenser with drying tube was charged with 12.4 g (0.05 mol) of 1,3-bis(3-aminopropyl)tetramethyldisiloxane, 18.1 (88.12 mmol) of tetramethylammonium hydroxide pentahydrate, and 30 ml of tetrahydrofuran. The mixture was heated under reflux in an inert gas atmosphere for 5 hours. A 250 ml three-neck round-bottom flask equipped with a magnetic stirrer, argon inlet, and condenser with drying tube The mixture was heated under reflux in an inert gas atmosphere for 5 hours

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 5 liters four-necked flask equipped with a stirrer, a thermometer, a gas-inlet tube, and a condenser were placed 1000 g (4.0 moles) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetra-methyldisiloxane having a gas chromatography purity of 98.4%, and 2,600 g of isopropanol. 360 g (9.9 moles) of hydrogen chloride gas was bubbled into the solution while stirring the mixture at room temperature. Recrystallization was conducted to obtain 1,250 g (yield: 97%) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which was an acid addition salt. In a 5 liters four-necked flask equipped with a stirrer Recrystallization

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 500 ml four-necked flask equipped with a stirrer, a thermometer, a condenser, and a dropping funnel was placed 24.9 g (0.1 mole) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane having a gas chromatography purity of 98.4%. 31.3 g (0.3 mole) of concentrated hydrochloric acid was dropwise added to the flask, and the resulting mixture was stirred at room temperature for 30 minutes. 300 g of isopropanol was added to the solution. The resulting mixture was heated under reduced pressure, and isopropanol was distilled off while conducting azeotropic distillation, to obtain a concentrated and dried product. The concentrated and dried product thus obtained was recrystallized from isopropanol to obtain 28.9 g (yield: 90%) of 1,3-bis(3-amino-propyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which is an acid addition salt. In a 500 ml four-necked flask equipped with a stirrer was distilled off distillation to obtain a concentrated The concentrated dried product thus obtained was recrystallized from isopropanol