3-chloropropyl(trimethoxy)silane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 267.6 g of a methanol solution of 22% sodium hydrogensulfide anhydride (1.05 mol) was put into an autoclave with an internal volume of 1 liter and the air was replaced by nitrogen. 0.3 mol of hydrogen sulfide was then blown in and the system was pressurized to 0.9 kgf/cm2 to oversaturate hydrogen sulfide. After heating the system up to 90° C., 198.7 g (1.0 mole) of 3-chloropropyltrimethoxy silane was dripped for 3 hours, and during the dripping, 0.1 mol of hydrogen sulfide was blown into the system so that the pressure in the system was kept at 3.5 kgf/cm2. After the dripping, the system was aged for 2 hour at 90° C., followed by cooling. By-product salts produced in the reaction were filtered away. The composition was analyzed by means of gas chromatography. 3-mercaptopropyltrimethoxy silane was obtained with a yield of 93.5%. by cooling By-product salts produced in the reaction were filtered away

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 267.6 g of a methanol solution of 22% sodium hydrogensulfide anhydride (1.05 mol) was put into an autoclave with an internal volume of 1 liter, and the air was replaced by nitrogen. 0.3 mol of hydrogen sulfide was then blown in and the system was pressurized to 0.9 kgf/cm2 to oversaturate hydrogen sulfide. After heating the system up to 70° C., 198.7 g (1.0 mole) of 3-chloropropyltrimethoxy silane was dripped for 3 hours, and, during the dripping, 0.05 mol of hydrogen sulfide was blown into the system so that the pressure in the system was kept at 2.5 kgf/cm2. After the dripping, the temperature was raised to 100° C. and the system was aged for 1 hour, followed by cooling. By-product salts produced in the reaction were filtered away. The composition was analyzed by means of gas chromatography. 3-mercaptopropyltrimethoxy silane was obtained with a yield of 94.1%. After the dripping, the temperature was raised to 100° C. by cooling By-product salts produced in the reaction were filtered away

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A one-liter, four-necked flask was equipped with a thermometer, a condensor, an inlet tube for nitrogen gas and an outlet tube for vent gases. Chloropropyltrimethoxysilane (198.72 g) was introduced into the flask, together with 50 g of anhydrrous 1,1,1-trichloroethane and 86.14 g of 1-(2-aminoethyl)- piperazine. The mixture was heated to 80° C. with continuous agitation for four hours and then cooled to room temperature. The reaction mixture was rapidly filtered to collect the 1-(2-aminoethyl)piperazine hydrochloride salt which had formed. The filtrate was distilled to yield 182 g of 1-[2-[3-(trimethoxysilyl)- propyl]aminoethyl]piperazine, bp 120°-143° C. at 10 mm Hg (69 kPa) as a pale yellow oil. The yield corresponded to 64% of theoretical. This material was used as an accelerator and adhesion promoter in the sealant compositions of this invention as detailed below in Example 5. A one-liter, four-necked flask was equipped with a thermometer cooled to room temperature The reaction mixture was rapidly filtered to collect the 1-(2-aminoethyl)piperazine hydrochloride salt which had formed The filtrate was distilled

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir: