dimethoxy(dimethyl)silane

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

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

Procedure: Under a nitrogen gas atmosphere, 5.00 g (9.11 mmol) of 2,7-dibromo-9,9-dioctylfluorene, 20 ml of diethyl ether and 10 ml of toluene were added to a 100 ml three-necked flask equipped with a reflux condenser and a dropping funnel. Under cooling by an ice bath, 6.2 ml (9.92 mmol) of a hexane solution of n-butyllithium (1.6 M) was added dropwise. As the butyllithium was added, the solution turned red. This solution was agitated “as is” for approximately 1 hour; then, 520 mg (4.33 mmol) of dimethoxydimethylsilane was added, and the resulting mixture was agitated and reacted all night. equipped with a reflux condenser and a dropping funnel Under cooling by an ice bath for approximately 1 hour the resulting mixture was agitated reacted all night

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

Procedure: Under a nitrogen atmosphere, dimethoxydimethylsilane (31) (1.0 ml, 7.0 mmol) was added to a reaction container, cooled down to 0° C., diethyl ether solution of 0.72M 3-(triallylsilyl)propylmagnesium bromide (24) (19.44 mL, 14 mmol) was added dropwise. After the dropwise adding, stirring was continued at room temperature for 5 hours. To the reaction mixture, water was added to stop the reaction, then 10% hydrochloric acid was added until the salt was completely dissolved. The obtained organic layer was separated and the obtained water layer was extracted with diethyl ether. The collected organic layer was washed each with saturated sodium bicarbonate aqueous solution and saturated saline solution in this order, dried over anhydrous magnesium sulfate, then filtered, concentrated under reduced pressure, obtaining {3-(triallylsilyl)propyl}(methoxy)dimethylsilane (32) represented by the following chemical reaction equation (yield: 1.5 g, yield (%): 72%). After the dropwise adding the reaction was completely dissolved The obtained organic layer was separated the obtained water layer was extracted with diethyl ether The collected organic layer was washed each with saturated sodium bicarbonate aqueous solution and saturated saline solution in this order dried over anhydrous magnesium sulfate filtered concentrated under reduced pressure

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

Conditions: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a pressure-resistant reactor, 23.3 kg of cyclohexane, 2.5 millimoles of N,N,N′,N′-tetramethyl ethylene diamine (herein below, referred to as TMEDA) and 1.55 kg of styrene were added and stirred at 40° C. Added thereto was 164.7 millimoles of n-butyl lithium, and while the temperature was increased to 50° C., the mixture was polymerized for 1 hour. The degree of polymerization conversion of styrene in this stage was 100%. Subsequently, 5.20 kg of isoprene was added to the reactor continuously over 1 hour while the temperature was controlled to maintain 50 to 60° C. After the addition of isoprene was finished, the mixture was polymerized for additional 1 hour. The degree of polymerization conversion of isoprene was 100%. Subsequently, 60.1 millimoles of dimethyl dimethoxysilane was added thereto as a coupling agent and the coupling reaction was performed for 2 hours to produce a styrene-isoprene-styrene block copolymer, which would be the block copolymer B. Next, 23.1 millimoles of methanol was added to the reactor to deactivate the active terminal of part of the styrene-isoprene block copolymer. After that, while the temperature was controlled such that it was kept at 50 to 60° C., 3.25 kg of styrene was continuously added over 1 hour. After the addition of styrene was completed, the polymerization was performed for additional 1 hour to produce a styrene-isoprene-styrene block copolymer, which would be the block copolymer A. The degree of polymerization conversion of styrene was 100%. After that, 329.4 millimoles of methanol was added as a polymerization terminator and mixed well to terminate the reaction. The amount of each reagent used for the reaction is shown in Table 1. Part of the reaction solution obtained was extracted and the weight average molecular weight of each block copolymer and block copolymer composition, the weight average molecular weight of each styrene polymer block, the weight average molecular weight of each isoprene polymer block, the content of the styrene unit in each block copolymer, the content of the styrene unit in the block copolymer composition, the vinyl bond content in the isoprene polymer block, and the weight ratio of each block copolymer were measured. The results are shown in Table 2. To 100 parts of the reaction solution obtained (containing 30 parts of polymer components), 0.3 part of 2,6-di-tert-butyl-p-cresol was added as an anti-oxidant and mixed well. The mixture solution was added dropwise in small portions to hot water heated to 85 to 95° C. to evaporate the solvent. Accordingly, the precipitates were obtained, pulverized, and dried with hot air (85° C.) to recover the block copolymer composition of Preparation example 1. Added while the temperature was increased to 50° C. the mixture was polymerized for 1 hour to maintain 50 to 60° C the mixture was polymerized for additional 1 hour as a coupling agent and the coupling reaction

Conditions: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 306 mg Of allyl chloride, 530 mol of dimethyldimethoxysilane, and 77 mg of toluene were placed in a glass reaction tube and 0.01 ml of acetic acid was added to this mixture. Then, 0.005 mol of a toluene solution of a 0-valent platinum complex of divinyltetramethyldisiloxane (platinum content: 0.4 wt %) was added to this mixture. The reaction tube was sealed and heated for 2 hours in an oil bath at 50° C. When the contents were analyzed by GC-MS following cooling, the conversion rate of allyl chloride was 100% and γ-chloropropylmethyldimethoxysilane was produced at a yield of 40%. was added to this mixture The reaction tube was sealed following cooling

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

Procedure: Under a nitrogen gas atmosphere, 5.00 g (9.11 mmol) of 2,7-dibromo-9,9-dioctylfluorene, 20 ml of diethyl ether and 10 ml of toluene were added to a 100 ml three-necked flask equipped with a reflux condenser and a dropping funnel. Under cooling by an ice bath, 6.2 ml (9.92 mmol) of a hexane solution of n-butyllithium (1.6 M) was added dropwise. As the butyllithium was added, the solution turned red. This solution was agitated “as is” for approximately 1 hour; then, 520 mg (4.33 mmol) of dimethoxydimethylsilane was added, and the resulting mixture was agitated and reacted all night. equipped with a reflux condenser and a dropping funnel Under cooling by an ice bath for approximately 1 hour the resulting mixture was agitated reacted all night

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

Procedure: Under a nitrogen atmosphere, dimethoxydimethylsilane (31) (1.0 ml, 7.0 mmol) was added to a reaction container, cooled down to 0° C., diethyl ether solution of 0.72M 3-(triallylsilyl)propylmagnesium bromide (24) (19.44 mL, 14 mmol) was added dropwise. After the dropwise adding, stirring was continued at room temperature for 5 hours. To the reaction mixture, water was added to stop the reaction, then 10% hydrochloric acid was added until the salt was completely dissolved. The obtained organic layer was separated and the obtained water layer was extracted with diethyl ether. The collected organic layer was washed each with saturated sodium bicarbonate aqueous solution and saturated saline solution in this order, dried over anhydrous magnesium sulfate, then filtered, concentrated under reduced pressure, obtaining {3-(triallylsilyl)propyl}(methoxy)dimethylsilane (32) represented by the following chemical reaction equation (yield: 1.5 g, yield (%): 72%). After the dropwise adding the reaction was completely dissolved The obtained organic layer was separated the obtained water layer was extracted with diethyl ether The collected organic layer was washed each with saturated sodium bicarbonate aqueous solution and saturated saline solution in this order dried over anhydrous magnesium sulfate filtered concentrated under reduced pressure