3-chloropropyl-dimethoxy-methylsilane

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: 33.4 g (417 mmol) of freshly distilled methylcyclopentadiene are added dropwise to a suspension of 10 g (417 mmol) of sodium hydride in 250 ml of absolute diethyl ether at RT over a period of one hour. 76.1 g of (3-chloropropyl)dimethoxy-methylsilane are subsequently added dropwise over a period of 30 minutes. The solution becomes warm during this process. After taking off the solvent, the mixture is fractionally distilled in an oil pump vacuum to give 78.9 g of (3-methylcyclopentadienylpropyl)dimethoxy-methylsilane (yield: 89%). The solution becomes warm during this process the mixture is fractionally distilled in an oil pump vacuum

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

実験手順: Starting with 182.7 g of chloropropylmethyldimethoxysilane and 79 g of 2-aminoethylpiperazine, the procedure described in Example 2 was used to prepare 75 g of the title compound, boiling point range 90°-110° C. at 5 mm Hg (34 kPa).

反応条件: temp:115.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Using the general procedure described in Example 1 a reactor was charged with 60 g (0.55 mole) of p-aminophenol, 43.28 g of a 50% by weight aqueous solution of sodium hydroxide (0.54 mole NaOH), 112 cc dimethylsulfoxide and 120 cc toluene. The resultant mixture was heated to the boiling point for six hours under a nitrogen atmosphere to remove all of the water present by azeotropic distillation. The reaction mixture was then allowed to cool to about 75° C., at which time 100.4 g (0.56 mole) of 3-chloropropyl methyldimethoxysilane was added dropwise while the reaction mixture was stirred. Following completion of the addition the reaction mixture was heated at 115° C. for about 16 hours, following which the mixture was allowed to cool and was filtered to remove any solid material. The solvents were then removed under a pressure of about 15 mm of mercury at a temperature of about 60° C. The pressure was then reduced to from 3 to 4 mm of mercury and the material boiling from 230° to 235° C. was removed. This fraction weighed 112 g, equivalent to a yield of 80% based on starting materials. Analysis by vapor phase chromatography indicated that the purity of the product was greater than 98%. The infrared and nuclear magnetic resonance spectra of the product were consistent with the proposed structure. to remove all of the water present by azeotropic distillation was added dropwise while the reaction mixture completion of the addition the reaction mixture to cool was filtered to remove any solid material The solvents were then removed under a pressure of about 15 mm of mercury at a temperature of about 60° C boiling from 230° to 235° C. was removed

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

実験手順: 33.4 g (417 mmol) of freshly distilled methylcyclopentadiene are added dropwise to a suspension of 10 g (417 mmol) of sodium hydride in 250 ml of absolute diethyl ether at RT over a period of one hour. 76.1 g of (3-chloropropyl)dimethoxy-methylsilane are subsequently added dropwise over a period of 30 minutes. The solution becomes warm during this process. After taking off the solvent, the mixture is fractionally distilled in an oil pump vacuum to give 78.9 g of (3-methylcyclopentadienylpropyl)dimethoxy-methylsilane (yield: 89%). The solution becomes warm during this process the mixture is fractionally distilled in an oil pump vacuum

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

実験手順: Starting with 182.7 g of chloropropylmethyldimethoxysilane and 79 g of 2-aminoethylpiperazine, the procedure described in Example 2 was used to prepare 75 g of the title compound, boiling point range 90°-110° C. at 5 mm Hg (34 kPa).

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

実験手順: Starting with 182.7 g of chloropropylmethyldimethoxysilane and 79 g of 2-aminoethylpiperazine, the procedure described in Example 2 was used to prepare 75 g of the title compound, boiling point range 90°-110° C. at 5 mm Hg (34 kPa).

反応条件: temp:115.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Using the general procedure described in Example 1 a reactor was charged with 60 g (0.55 mole) of p-aminophenol, 43.28 g of a 50% by weight aqueous solution of sodium hydroxide (0.54 mole NaOH), 112 cc dimethylsulfoxide and 120 cc toluene. The resultant mixture was heated to the boiling point for six hours under a nitrogen atmosphere to remove all of the water present by azeotropic distillation. The reaction mixture was then allowed to cool to about 75° C., at which time 100.4 g (0.56 mole) of 3-chloropropyl methyldimethoxysilane was added dropwise while the reaction mixture was stirred. Following completion of the addition the reaction mixture was heated at 115° C. for about 16 hours, following which the mixture was allowed to cool and was filtered to remove any solid material. The solvents were then removed under a pressure of about 15 mm of mercury at a temperature of about 60° C. The pressure was then reduced to from 3 to 4 mm of mercury and the material boiling from 230° to 235° C. was removed. This fraction weighed 112 g, equivalent to a yield of 80% based on starting materials. Analysis by vapor phase chromatography indicated that the purity of the product was greater than 98%. The infrared and nuclear magnetic resonance spectra of the product were consistent with the proposed structure. to remove all of the water present by azeotropic distillation was added dropwise while the reaction mixture completion of the addition the reaction mixture to cool was filtered to remove any solid material The solvents were then removed under a pressure of about 15 mm of mercury at a temperature of about 60° C boiling from 230° to 235° C. was removed

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 306 mg of allyl chloride, 530 mol of dimethyldiethoxysilane, and 77 mg of toluene were placed in a glass reaction tube. 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 19.7%. The reaction tube was sealed following cooling

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 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

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

実験手順: 33.4 g (417 mmol) of freshly distilled methylcyclopentadiene are added dropwise to a suspension of 10 g (417 mmol) of sodium hydride in 250 ml of absolute diethyl ether at RT over a period of one hour. 76.1 g of (3-chloropropyl)dimethoxy-methylsilane are subsequently added dropwise over a period of 30 minutes. The solution becomes warm during this process. After taking off the solvent, the mixture is fractionally distilled in an oil pump vacuum to give 78.9 g of (3-methylcyclopentadienylpropyl)dimethoxy-methylsilane (yield: 89%). The solution becomes warm during this process the mixture is fractionally distilled in an oil pump vacuum