trimethoxy(methyl)silane

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

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

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

Procedure: A 500 ml 5-neck round-bottom flask, rendered inert with nitrogen and equipped with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 50 g (0.36 mol) of methyl-trimethoxysilane (available commercially from Wacker Chemie AG), 8.8 g (0.04 mol) of 3,3,3-trifluoro-propyltrimethoxysilane (available commercially from Fluka), and 39.7 g of Isopar E (isoparaffinic hydro-carbon mixture having a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 350 rpm, a solution of 17.2 g of potassium hydroxide (85% strength, available commercially from AppliChem) (0.26 mol of potassium hydroxide) and 15.3 g of demineralized water is metered in over 12 minutes. During this metered addition, the mixture heats up to 67° C. The mixture is heated to boiling temperature (70° C.). The distillate separates out as the bottom phase in the water separator. Up to a boiling temperature of 119° C., 48.5 g of colorless, slightly turbid distillate accumulate. The suspension which remains is subsequently evaporated to dryness with stirring under a full oil-pump vacuum (5 hPa) to 70° C. This gives 45.9 g of fine, white, free-flowable powder with a solids content of 99.7% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this powder exhibits no precipitation even after being stored at room temperature for two weeks in the absence of air. A 500 ml 5-neck round-bottom flask, rendered inert with nitrogen equipped with paddle stirrer with reflux condenser is metered in over 12 minutes During this metered addition heats up to 67° C The suspension which remains is subsequently evaporated to dryness with stirring under a full oil-pump vacuum (5 hPa) to 70° C at 160° C. A 50% strength aqueous solution prepared with this powder no precipitation even after being stored at room temperature for two weeks in the absence of air

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

Procedure: A 500 ml 5-neck round-bottom flask, rendered inert with nitrogen and equipped with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 70 g (0.5 mol) of methyl-trimethoxysilane (available commercially from Wacker Chemie AG), 6 g (0.05 mol) of trimethylmethoxysilane (prepared in the laboratory by reacting trimethyl-chlorosilane with methanol), and 98.6 g of Isopar E (isoparaffinic hydrocarbon mixture having a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 300 rpm, a solution of 40.5 g of 50% strength aqueous potassium hydroxide solution (0.36 mol of potassium hydroxide) and 3.2 g of demineralized water is metered in over 6 minutes. During this metered addition, the mixture heats up to 63° C. The mixture is heated to boiling temperature (70° C.). The distillate separates out as the bottom phase in the water separator. Up to a boiling temperature of 118° C., 60.3 g of colorless, slightly turbid distillate are accumulated, and—according to analysis by gas chromatography—contains 84 area % of methanol, 10.8 area % of water, 3.3 area % of Isopar E, and 0.8 area % of trimethylmethoxysilane. The suspension which remains is subsequently evaporated to dryness with stirring under a full oil-pump vacuum (5 hPa) to 70° C. This gives 55.9 g of fine, white, free-flowable powder with a solids content of 99.9% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this powder exhibits no precipitation even after being stored at room temperature for two weeks in the absence of air. A 500 ml 5-neck round-bottom flask, rendered inert with nitrogen equipped with paddle stirrer with reflux condenser prepared in the laboratory is metered in over 6 minutes During this metered addition heats up to 63° C The suspension which remains is subsequently evaporated to dryness with stirring under a full oil-pump vacuum (5 hPa) to 70° C at 160° C. A 50% strength aqueous solution prepared with this powder no precipitation even after being stored at room temperature for two weeks in the absence of air

Conditions: temp:66.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 500 ml 5-neck glass flask, rendered inert with nitrogen and equipped with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 50 g (0.36 mol) of methyl-trimethoxysilane (available commercially from Wacker Chemie AG) and 31.8 g of Isopar E (isoparaffinic hydro-carbon mixture having a boiling range of 113-143° C., available commercially from ExxonMobil). Accompanied by stirring at 300 rpm, a solution of 31.8 g of 50% strength aqueous potassium hydroxide solution (0.23 mol of potassium hydroxide) and 2.1 g (0.117 mol) of demineralized water is metered in over 10 minutes. During this metered addition, the mixture heats up to 58° C. It is heated at reflux (66° C.) for an hour and then the distillate is switched to the water separator, which is filled to the brim with Isopar E. Up to a boiling temperature of 118° C., 49 g of colorless, slightly turbid distillate are accumulated, and—according to analysis by gas chromatography—contains 84 area% of methanol, 14 area% of water, and 2 area% of Isopar E. During the distillation, a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension. All of the volatile constituents are distilled off with stirring at an oil bath temperature of 70° C. under 5 hPa. This gives 37.3 g of fine, white, free-flowable powder with a solids content of 99.5% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this powder exhibits no precipitation even after being stored at room temperature for two weeks in the absence of air. The minimum ignition energy was determined on a powder prepared analogously: up to the maximum possible ignition energy setting of 10 J, there was no ignition in the fluidized dust. A 500 ml 5-neck glass flask, rendered inert with nitrogen equipped with paddle stirrer with reflux condenser is metered in over 10 minutes During this metered addition heats up to 58° C It is heated is filled to the brim with Isopar E During the distillation a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension All of the volatile constituents are distilled off with stirring at an oil bath temperature of 70° C. under 5 hPa at 160° C. A 50% strength aqueous solution prepared with this powder no precipitation even after being stored at room temperature for two weeks in the absence of air prepared analogously

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

Procedure: A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 27 g (0.198 mol) of methyltrimethoxysilane (available commercially from Wacker Chemie AG), 3.9 g (0.02) of n-propyl(methyl)diethoxysilane (prepared in the laboratory by reacting n-propyl(methyl)dichlorosilane with ethanol) and 20 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 350 rpm, a solution of 12.4 g (0.188 mol) of potassium hydroxide (85% form, available commercially from AppliChem) in 7.9 g (0.44 mol) of demineralized water is metered in over 12 minutes. The mixture heats up to 48° C. It is heated to boiling temperature. The distillate separates off as the bottom phase in the water separator. Up to a boiling temperature of 95° C., 19.4 g of colorless, slightly turbid distillate accumulate, containing—according to analysis by gas chromatography—78.5% of methanol, 7.5% of ethanol, 3.5% of water, and 8.2% of Isopar E. The bottom phase is drained off from the water separator, which is made up completely with Isopar E again, and water is removed in circulation at a boiling temperature of up to 131° C. This produces 6.2 g of distillate as bottom phase, which according to GC analysis contains 46.9% of methanol, 4.7% of ethanol, and 48.4% of water. During the distillation, a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension. 10 g of cyclohexane are added and the suspension is filtered through a Beco KD3 filter plate in a pressure suction filter, and nitrogen is passed through to constant weight. This gives 21.4 g of fine, white, free-flowable powder with a solids content of 99.5% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air. A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer with reflux condenser prepared in the laboratory is metered in over 12 minutes heats up to 48° C It is heated water is removed in circulation at a boiling temperature of up to 131° C During the distillation a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension 10 g of cyclohexane are added the suspension is filtered through a Beco KD3 filter plate in a pressure suction filter at 160° C. A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air

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

Procedure: A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 30 g (0.22 mol) of methyltrimethoxysilane (available commercially from Wacker Chemie AG) and 50 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 350 rpm, a solution of 8.7 g (0.13 mol) of potassium hydroxide (85% form, available commercially from AppliChem) in 9.1 g (0.5 mol) of demineralized water is metered in over 12 minutes. The mixture heats up to 50° C. It is heated to boiling temperature and the stirrer speed is reduced to 50 rpm as soon as distillation begins. The distillate separates off as the bottom phase in the water separator. Up to a boiling temperature of 119° C., 25.4 g of clear colorless distillate accumulate, containing—according to analysis by gas chromatography—80.4% of methanol, 18.4% of water, and 1% of Isopar E. During the distillation, a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension. The suspension is filtered through a Beco KD3 filter plate in a pressure suction filter, and nitrogen is passed through until the weight is constant. This gives 19.8 g of fine, white, free-flowable powder with a solids content of 100% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air. A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer with reflux condenser is metered in over 12 minutes heats up to 50° C It is heated soon as distillation Up to a boiling temperature of 119° C., 25.4 g of clear colorless distillate accumulate, containing—according to analysis by gas chromatography—80.4% of methanol, 18.4% of water, and 1% of Isopar E During the distillation a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension The suspension is filtered through a Beco KD3 filter plate in a pressure suction filter at 160° C. A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air

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

Procedure: A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 50 g (0.367 mol) of methyltrimethoxysilane (available commercially from Wacker Chemie AG) and 65 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 300 rpm, a solution of 15.4 g (0.23 mol) of potassium hydroxide (85% form, available commercially from AppliChem) in 14.9 g (0.826 mol) of demineralized water is metered in over 12 minutes. The reaction mixture is heated to boiling temperature and the stirrer speed is reduced to 50 rpm as soon as distillation begins. The distillate separates off as the bottom phase in the water separator. Up to a boiling temperature of 85° C., 34.4 g of clear colorless distillate accumulate, containing—according to analysis by gas chromatography—87.8% of methanol, 4.9% of water, and 5.7% of Isopar E. The bottom phase is drained from the water separator, which is filled again completely with Isopar E, and water is removed in circulation up to a boiling temperature of 118° C. This produces 10.8 g of distillate as the bottom phase, containing—according to GC analysis—50.2% of methanol and 49.7% of water. The hydrolysis of the methoxy radicals in the methyltrimethoxysilane is therefore quantitative. During the distillation, a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension. The suspension is filtered through a Beco KD3 filter plate in a pressure suction filter, and nitrogen is passed through until the weight is constant. This gives 38 g of fine, white, free-flowable powder with a solids content of 99.7% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air. A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer with reflux condenser is metered in over 12 minutes The reaction mixture is heated soon as distillation Up to a boiling temperature of 85° C., 34.4 g of clear colorless distillate accumulate, containing—according to analysis by gas chromatography—87.8% of methanol, 4.9% of water, and 5.7% of Isopar E is filled again completely with Isopar E, and water is removed in circulation up to a boiling temperature of 118° C This produces 10.8 g of distillate as the bottom phase, containing—according The hydrolysis of the methoxy radicals in the methyltrimethoxysilane During the distillation a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension The suspension is filtered through a Beco KD3 filter plate in a pressure suction filter at 160° C. A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air

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

Procedure: A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 75 g (0.55 mol) of methyltrimethoxysilane (available commercially from Wacker Chemie AG) and 65 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 350 rpm, a solution of 30.9 g (0.47 mol) of potassium hydroxide (85% form, available commercially from AppliChem) in 19.8 g of demineralized water is metered in over 10 minutes. In the course of this metered addition, the reaction mixture heats up to 69° C. It is brought by further heating to boiling temperature, and the stirrer speed is reduced to 50 rpm. The distillate separates off as the bottom phase in the water separator. Up to a boiling temperature of 121° C., 64.9 g of clear colorless distillate accumulate, containing—according to analysis by gas chromatography—83.3% of methanol, 14.6% of water, and 1.7% of Isopar E. The hydrolysis of the methoxy radicals in the methyltrimethoxysilane is therefore quantitative. During the distillation, a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension. The suspension is filtered through a Beco KD3 filter plate in a pressure suction filter, and nitrogen is passed through until the weight is constant. This gives 61.1 g of fine, white, free-flowable powder with a solids content of 100% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air. A 500 ml 5-neck round-bottom flask, inertized with nitrogen and fitted with paddle stirrer with reflux condenser is metered in over 10 minutes In the course of this metered addition heats up to 69° C by further heating During the distillation a pastelike white solid separates out in the reaction mixture, and breaks down increasingly into fine particles and forms a suspension The suspension is filtered through a Beco KD3 filter plate in a pressure suction filter at 160° C. A 50% strength aqueous solution prepared with this solid exhibits no precipitation even after storage at room temperature for two weeks in the absence of air

Conditions: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The 22 ml Hastelloy-C pressure reactor of Example 3 was charged with 0.056 g (0.12 mol) of Ni(SC12H25)2, 5.0 g (47.2 mmol) of methyldimethoxysilane, 5.0 g (86.2 mmol) of acetone, and 0.5 g of dodecane as internal standard. The mixture was warmed to 130° C. and maintained at that temperature for 0.5 hours. After cooling, and venting off the hydrogen gas formed during the course of the reaction, gc analysis showed the presence of 1.12 g (22%) of starting methyldimethoxysilane, 0.85 g (13%) of methyltrimethoxysilane, 1.27 g (17%) of methyldimethoxyisopropoxy silane, and 3.64 g or a 62% yield of methyldimethoxyisopropenoxysilane. maintained at that temperature for 0.5 hours After cooling formed during the course of the reaction, gc analysis

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

Procedure: Si(O-n-C3H7)4; Si(O—isoC3H7)4; Si(OC2H4OCH3)4; CH3Si(OCH3)3; CH2═CHSi(OCH3)3; CH3Si(OC2H4OCH3)3; ClCH2Si(OC2H5)3; CH2═CHSi(OC2H4OCH3)3.

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