3-trimethoxysilylpropan-1-amine

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:; See reaction.notes.procedure_details.

実験手順: A mixture of 5.40 g of 3-aminopropyltrimethoxysilane, 6.80 g of hexanedioldiacrylate, 19.0 g of trimethylolpropane triacrylate, and 57.9 g of isopropanol is stirred at room temperature for 72 hours. To the mixture, 1.15 g of acetic acid is added, and the mixture is stirred for 5 minutes. Next, 56.2 g of NALCO 1034A is added under vigorous agitation. The resulting mixture is stirred at room temperature for 1 hour. 0.34 g of a solution of EBECRYL 1360 (50% by weight in PM glycol ether) and 1.80 g of DAROCUR 1173 are added. The resulting coating composition is stirred for an additional 30 minutes to ensure mixing. the mixture is stirred for 5 minutes The resulting mixture is stirred at room temperature for 1 hour The resulting coating composition is stirred for an additional 30 minutes to ensure mixing

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

実験手順: A mixture of 9.94 g of 3-aminopropyltrimethoxysilane and 15.4 g of hexanedioldiacrylate is stirred at room temperature for 3 hours. To the mixture, 28.5 g of PM glycol ether is added. The resulting mixture is stirred at room temperature for 1 minute. Then, 1.73 g of acrylic acid is added, and the mixture is stirred for 5 minutes. The mixture is diluted by adding 106.7 g of isopropanol. Next, 84.4 g of OG401-31 and 34.7 g of NALCO 1034A are added under vigorous agitation. The resulting mixture is stirred at room temperature for 1 hour. 0.74 g of a solution of EBECRYL 1360 (50% by weight in PM glycol ether), 3.98 g of DAROCUR 1173, and 64.8 g of n-butyl acetate are added. The resulting coating composition is stirred for an additional 30 minutes to ensure mixing. The resulting mixture is stirred at room temperature for 1 minute the mixture is stirred for 5 minutes The mixture is diluted The resulting mixture is stirred at room temperature for 1 hour The resulting coating composition is stirred for an additional 30 minutes to ensure mixing

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

実験手順: A mixture of 11.74 g of (3-(trimethoxysilyl)propyl)amine (0.0654 mol) and of 9.9 g of diisopropylcarbodiimide (0.0785 mol, 20% excess) was heated for 6 h 30 min at 80° C. Analysis by GC then showed an amine conversion of greater than 97%. The final colorless mixture was evaporated to dryness at 100° C. under 2 mbar for 2 h to give 22.5 g of a colorless, low-viscosity liquid corresponding to the expected guanidine. The final colorless mixture was evaporated to dryness at 100° C. under 2 mbar for 2 h

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3-Aminopropyltrimethoxysilane (11.05 g, 61.7 mmol) and methanol (20 ml) are stirred together for 30 minutes at room temperature. To the mixture is added 41.46 g (482 mmol) of methyl acrylate. The reaction mixture is heated overnight in a 30° C. oil bath. The reaction mixture is concentrated at reduced pressure to give 21.50 g of crude methyl 3-[(2-methoxycarbonylethyl)-(3-trimethoxysilylpropyl)amino]propionate, a yellow viscous oil. A mixture of the crude product, 1-[4-(2-hydroxyethyoxy)phenyl]-2-hydroxy-2-methylpropan-1-one (26.85 g, 119.7 mmol) and 1,2-dimethoxyethane (80 ml) is heated in an oil bath at 85° (bath temperature). Zirconium(IV) acetylacetonate (1.16 g, 2.38 mmol) is added, and the mixture is stirred at 85° C. overnight and then at room temperature for 24 hours. Solvent is evaporated, and approximately one-half of the crude product is passed through a silica gel column with 5:1 chloroform:methanol as eluent to obtain 15.74 g of the title compound, a yellow semisolid product. The reaction mixture is concentrated at reduced pressure

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 77.4 g 3-(amino)propyltrimethoxysilane, 43.7 g triethylamine and 25 mg di-tert.-butyl-p-cresol were dissolved under argon in 500 ml dichloromethane. 45.1 g methacryloyl chloride was slowly added dropwise at −5° C. within 1 h, and the whole was then stirred for 1 h at 0° C. The precipitated hydrochloride was filtered off and washed with dichloromethane. The volatile constituents were removed at 40° C. under reduced pressure using the rotary evaporator. A yellow liquid with precipitated solid (hydrochloride) remained. The precipitation of the hydrochloride was completed by adding 150 ml diethyl ether, the precipitate was filtered off and the filtrate concentrated at 40° C. using a rotary evaporator with introduction of dry air. The brownish liquid was freed of residual volatile constituents at 4×10−2 mbar, and the raw product (104.2 g) was distilled at a pressure of 6×10−4 mbar. The product had a boiling point of 123-125° C. 76.4 g of product was obtained as yellowish, clear liquid. The precipitated hydrochloride was filtered off washed with dichloromethane The volatile constituents were removed at 40° C. under reduced pressure the rotary evaporator A yellow liquid with precipitated solid (hydrochloride) The precipitation of the hydrochloride by adding 150 ml diethyl ether the precipitate was filtered off the filtrate concentrated at 40° C. a rotary evaporator with introduction of dry air the raw product (104.2 g) was distilled at a pressure of 6×10−4 mbar

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

実験手順: This compound was prepared according to the method described in the previous examples using 3-aminopropyltrimethoxysilane (17.9 g, 100 mmole), paraformaldehade (6.3 g, 210 mmole), 2-allyl-phenol (13.4 g, 0.1 mmole), and toluene (200 ml). The final product was obtained as a slightly yellow, mobile liquid. The yield was 94% of theory. This compound was prepared

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

実験手順: This compound was prepared according to the method described in previous examples using 3-aminopropyltrimethoxysilane (17.9 g, 100 mmole), paraformaldehyde (6.3 g, 210 mmole), 1-naphthol (14.4 g, 100 mmole), and toluene (200 ml). The final product was obtained as a viscous liquid. The yield was 80% of theory. This compound was prepared

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

実験手順: 13.57 g 2,2-dimethyl-3-dimethylaminopropanal, 7.45 g 2-propanamine and 17.93 g 3-aminopropyltrimethoxysilane were reacted according to the general manufacturing procedure (iminosilanes). The product was distilled after manufacture in order to remove oligomer portions. Yield: 28.4 g of a clear, colorless oil having an amine content of 6.61 mmol N/g and a purity of 95%. The product was distilled after manufacture in order to remove oligomer portions

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

実験手順: Example 1 was repeated except that the 41 grams of triethoxy silane was replaced with 30.6 grams of trimethoxy silane (0.25 mole) and toluene was used as a solvent instead of p-xylene, with other conditions remaining the same. After the completion of the reaction, the reaction mixture was subjected to gas chromatography analysis. It was found that gamma-aminopropyl trimethoxy silane was obtained in a yield of 70% on an allylamine basis, while the yield of beta-amminopropyl trimethoxy silane was 0.9% on an a trimethoxy silane basis. After the completion of the reaction