N-ethyl-2-methyl-3-trimethoxysilylpropan-1-amine

Conditions: temp:88.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 500 gallon reactor were added 489 kg (4.94 kmols) of N-ethylmethallylamine and 1425 g of platinum catalyst. The resulting solution was heated to 88° C. and 725 kg (5.94 kmols) of trimethoxysilane were added at such a rate to keep the temperature under 105° C. After addition was complete, the contents were heated to 110° C. for one hr. The low boiling byproducts were then removed by overhead stripping. The mixture was then cooled and approximately 60 L of methanol were added, and the reaction mixture was agitated at 50° C. for 1 hour before stripping the excess methanol. The resulting crude material (>97% purity) was then transferred from the reactor. The process was repeated without cleanup of the reactor to yield a combined total of 1638 kg (7.41 kmol) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. under 105° C After addition the contents were heated to 110° C. for one hr The low boiling byproducts were then removed by overhead stripping The mixture was then cooled approximately 60 L of methanol were added

Conditions: temp:68.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A one-liter three-neck round bottom flask was equipped with a magnetic stir bar, standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler. The flask was charged with 220 g (1.80 mols) of trimethoxysilane and heated to 60° C. at which temperature 0.25 ml of platinum tris(divinyltetramethyl disiloxane)diplatinum (0) (5% Pt content in toluene—referred to as Pt catalyst throughout these examples) was added. The solution was further heated to 68° C. and dropwise addition of 150 g (1.52 mols) of N-ethylmethallylamine was then conducted over a period of 45 minutes. After addition, the contents were heated to 90° C. and maintained at this temperature for 1 hr. The temperature was then increased to 105° C. and held for 4.5 hrs. Upon completion of the reaction, the mixture was cooled to room temperature and 16 g (0.5 mols) of methanol were added and gently heated prior to distillation. Final purification via vacuum distillation yielded 273 g (1.24 mols) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. The product (b.p. 98-100° C. at 12 mm Hg) was characterized via GC/MS. The isolated yield was 82%. Product structure was supported by GC/MS analysis. A one-liter three-neck round bottom flask was equipped with a magnetic stir bar standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler was added After addition the contents were heated to 90° C. maintained at this temperature for 1 hr The temperature was then increased to 105° C. held for 4.5 hrs Upon completion of the reaction the mixture was cooled to room temperature gently heated to distillation Final purification via vacuum distillation

Conditions: temp:88.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 500 gallon reactor were added 489 kg (4.94 kmols) of N-ethylmethallylamine and 1425 g of platinum catalyst. The resulting solution was heated to 88° C. and 725 kg (5.94 kmols) of trimethoxysilane were added at such a rate to keep the temperature under 105° C. After addition was complete, the contents were heated to 110° C. for one hr. The low boiling byproducts were then removed by overhead stripping. The mixture was then cooled and approximately 60 L of methanol were added, and the reaction mixture was agitated at 50° C. for 1 hour before stripping the excess methanol. The resulting crude material (>97% purity) was then transferred from the reactor. The process was repeated without cleanup of the reactor to yield a combined total of 1638 kg (7.41 kmol) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. under 105° C After addition the contents were heated to 110° C. for one hr The low boiling byproducts were then removed by overhead stripping The mixture was then cooled approximately 60 L of methanol were added

Conditions: temp:68.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A one-liter three-neck round bottom flask was equipped with a magnetic stir bar, standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler. The flask was charged with 220 g (1.80 mols) of trimethoxysilane and heated to 60° C. at which temperature 0.25 ml of platinum tris(divinyltetramethyl disiloxane)diplatinum (0) (5% Pt content in toluene—referred to as Pt catalyst throughout these examples) was added. The solution was further heated to 68° C. and dropwise addition of 150 g (1.52 mols) of N-ethylmethallylamine was then conducted over a period of 45 minutes. After addition, the contents were heated to 90° C. and maintained at this temperature for 1 hr. The temperature was then increased to 105° C. and held for 4.5 hrs. Upon completion of the reaction, the mixture was cooled to room temperature and 16 g (0.5 mols) of methanol were added and gently heated prior to distillation. Final purification via vacuum distillation yielded 273 g (1.24 mols) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. The product (b.p. 98-100° C. at 12 mm Hg) was characterized via GC/MS. The isolated yield was 82%. Product structure was supported by GC/MS analysis. A one-liter three-neck round bottom flask was equipped with a magnetic stir bar standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler was added After addition the contents were heated to 90° C. maintained at this temperature for 1 hr The temperature was then increased to 105° C. held for 4.5 hrs Upon completion of the reaction the mixture was cooled to room temperature gently heated to distillation Final purification via vacuum distillation

Conditions: temp:68.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A one-liter three-neck round bottom flask was equipped with a magnetic stir bar, standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler. The flask was charged with 220 g (1.80 mols) of trimethoxysilane and heated to 60° C. at which temperature 0.25 ml of platinum tris(divinyltetramethyl disiloxane)diplatinum (0) (5% Pt content in toluene—referred to as Pt catalyst throughout these examples) was added. The solution was further heated to 68° C. and dropwise addition of 150 g (1.52 mols) of N-ethylmethallylamine was then conducted over a period of 45 minutes. After addition, the contents were heated to 90° C. and maintained at this temperature for 1 hr. The temperature was then increased to 105° C. and held for 4.5 hrs. Upon completion of the reaction, the mixture was cooled to room temperature and 16 g (0.5 mols) of methanol were added and gently heated prior to distillation. Final purification via vacuum distillation yielded 273 g (1.24 mols) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. The product (b.p. 98-100° C. at 12 mm Hg) was characterized via GC/MS. The isolated yield was 82%. Product structure was supported by GC/MS analysis. A one-liter three-neck round bottom flask was equipped with a magnetic stir bar standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler was added After addition the contents were heated to 90° C. maintained at this temperature for 1 hr The temperature was then increased to 105° C. held for 4.5 hrs Upon completion of the reaction the mixture was cooled to room temperature gently heated to distillation Final purification via vacuum distillation

Conditions: temp:88.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 500 gallon reactor were added 489 kg (4.94 kmols) of N-ethylmethallylamine and 1425 g of platinum catalyst. The resulting solution was heated to 88° C. and 725 kg (5.94 kmols) of trimethoxysilane were added at such a rate to keep the temperature under 105° C. After addition was complete, the contents were heated to 110° C. for one hr. The low boiling byproducts were then removed by overhead stripping. The mixture was then cooled and approximately 60 L of methanol were added, and the reaction mixture was agitated at 50° C. for 1 hour before stripping the excess methanol. The resulting crude material (>97% purity) was then transferred from the reactor. The process was repeated without cleanup of the reactor to yield a combined total of 1638 kg (7.41 kmol) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. under 105° C After addition the contents were heated to 110° C. for one hr The low boiling byproducts were then removed by overhead stripping The mixture was then cooled approximately 60 L of methanol were added

Conditions: temp:68.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A one-liter three-neck round bottom flask was equipped with a magnetic stir bar, standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler. The flask was charged with 220 g (1.80 mols) of trimethoxysilane and heated to 60° C. at which temperature 0.25 ml of platinum tris(divinyltetramethyl disiloxane)diplatinum (0) (5% Pt content in toluene—referred to as Pt catalyst throughout these examples) was added. The solution was further heated to 68° C. and dropwise addition of 150 g (1.52 mols) of N-ethylmethallylamine was then conducted over a period of 45 minutes. After addition, the contents were heated to 90° C. and maintained at this temperature for 1 hr. The temperature was then increased to 105° C. and held for 4.5 hrs. Upon completion of the reaction, the mixture was cooled to room temperature and 16 g (0.5 mols) of methanol were added and gently heated prior to distillation. Final purification via vacuum distillation yielded 273 g (1.24 mols) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. The product (b.p. 98-100° C. at 12 mm Hg) was characterized via GC/MS. The isolated yield was 82%. Product structure was supported by GC/MS analysis. A one-liter three-neck round bottom flask was equipped with a magnetic stir bar standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler was added After addition the contents were heated to 90° C. maintained at this temperature for 1 hr The temperature was then increased to 105° C. held for 4.5 hrs Upon completion of the reaction the mixture was cooled to room temperature gently heated to distillation Final purification via vacuum distillation