3-triethoxysilylpropan-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:; See reaction.notes.procedure_details.

実験手順: To a degassed solution of 1-iodo-3,5-bistrifluoromethylbenzene (10.0 g, 29.4 mmol), anilinium hypophosphite (5.62 g, 35.3 mmol) and 3-aminopropyl triethoxysilane (7.81 g, 35.3 mmol) in anhydrous acetonitrile (200 mL) were added palladium acetate (132 mg, 0.588 mmol, 2 mol %) and 1,3-bis(diphenylphosphino)propane (267 mg, 0.647 mol, 2.2 mol %). The mixture was heated under reflux overnight, then cooled down to room temperature, diluted with ethyl acetate and hydrochloric acid (1M), and partitioned. The aqueous layer was further extracted with ethyl acetate and the combined extracts were washed with aqueous sodium hydrogen carbonate and brine, and dried over sodium sulfate. The volatiles were removed in vacuo, and the residue was purified by column chromatography using 30 to 70% ethyl acetate in petroleum ether to afford compound AZ3 (4.65 g) as a cloudy oil in 52% yield. The mixture was heated under reflux overnight partitioned The aqueous layer was further extracted with ethyl acetate the combined extracts were washed with aqueous sodium hydrogen carbonate and brine dried over sodium sulfate The volatiles were removed in vacuo the residue was purified by column chromatography to afford compound AZ3 (4.65 g) as a cloudy oil in 52% yield

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

実験手順: To a degassed mixture of 4-fluoro-1-iodo-benzene (25.0 g, 112.6 mmol), anilinium hypophosphite (21.5 g, 135.1 mmol) and 3-aminopropyl triethoxysilane (24.9 g, 135.1 mmol) in anhydrous acetonitrile (750 mL) were added palladium acetate (560 mg, 2.48 mmol) and 1,3-bis(diphenylphosphino)propane (1.02 g, 2.48 mmol). The mixture was heated under reflux overnight, then cooled down to room temperature, and the volatiles were removed in vacuo. The residue was diluted with ethyl acetate and hydrochloric acid (1M) and partitioned. The aqueous layer was further extracted with ethyl acetate and the combined extracts were washed with aqueous sodium hydrogen carbonate and brine. The volatiles were removed in vacuo, then the residue was purified by column chromatography using 50 to 100% ethyl acetate in petroleum ether, affording compound AZ2 (10.1 g) as a dark orange oil in 48% yield. The mixture was heated under reflux overnight the volatiles were removed in vacuo The residue was diluted with ethyl acetate and hydrochloric acid (1M) partitioned The aqueous layer was further extracted with ethyl acetate the combined extracts were washed with aqueous sodium hydrogen carbonate and brine The volatiles were removed in vacuo the residue was purified by column chromatography affording compound AZ2 (10.1 g) as a dark orange oil in 48% yield

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

実験手順: To a degassed solution of 4-iodobenzotrifluoride (4.70 g, 17.2 mmol), anilinium hypophosphite (3.51 g, 22.1 mmol), and 3-aminopropyl triethoxysilane (4.88 g, 22.1 mmol) in anhydrous acetonitrile (110 mL) were added palladium acetate (82.5 mg, 0.367 mmol, 2 mol %) and 1,3-bis(diphenylphosphino)propane (167 mg, 0.404 mol, 2.2 mol %). The mixture was heated under reflux for 32 hrs, then cooled down to room temperature, diluted with ethyl acetate and hydrochloric acid (IM) and partitioned. The aqueous layer was further extracted with ethyl acetate, and the combined extracts were washed with aqueous sodium hydrogen carbonate and brine and dried over magnesium sulfate. The solvent was removed in vacuo and the residue was purified by column chromatography using 25 to 100% ethyl acetate in petroleum ether. Further purification by distillation afforded compound AZ1 (1.14 g) in 28% yield. The mixture was heated under reflux for 32 hrs partitioned The aqueous layer was further extracted with ethyl acetate the combined extracts were washed with aqueous sodium hydrogen carbonate and brine dried over magnesium sulfate The solvent was removed in vacuo the residue was purified by column chromatography Further purification by distillation afforded compound AZ1 (1.14 g) in 28% yield

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

実験手順: 43 g (0.25 mol) 3-aminopropyl triethoxysilane in 40 ml anhydrous acetonitrile are added dropwise accompanied by ice-cooling to 92 g (0.5 mol) 2-acryloyloxyethyl methacrylate in 85 ml acetonitrile. After 48 h stirring at room temperature, the aminosilane has completely reacted. The solvent is evaporated off accompanied by the introduction of air at reduced pressure at the rotary evaporator at maximally 46° C. 132.2 g (98% yield) of a lightly-coloured clear oily liquid are obtained. The solvent is evaporated off accompanied by the introduction of air at reduced pressure at the rotary evaporator at maximally 46° C

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

実験手順: The adequate amount of 3-aminopropyltriethoxysilane (APTES) is dissolved in ethanol, and the adequate amount of fluorescein isothiocyanate (FITC) is added therein to mix well to form a ethanol solution of FITC-silane. to mix well

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

実験手順: Preferably, Route A can be used. A chloromethylated ligand can be prepared, for example, by reacting 8-hydroxyquinoline with formaldehyde and hydrochloric acid. That derivative is further reacted with γ-aminopropyltriethoxysilane in the presence of trimethylchlorosilane and triethylamine and nitrobenzene. Next, the prepared organosilicon derivative is reacted with the support to obtain hydroxyquinoline modified silica gel. A sample of this sequence of reactions is described in further detail in Example 2 below.

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

実験手順: 3-Aminopropyltriethoxysilane (22.14 g, 0.100 mol) is added to a solution of 26.03 g (0.100 mol) of 6-(4-methoxy-benzoyl)-7-oxa-bicyclo[4.2.0]octan-8-one in methylene chloride. The reaction mixture is heated at reflux for several hours and monitored by thin layer chromatography. Upon completion of the reaction, solvent is evaporated to obtain the title compound. The reaction mixture is heated at reflux for several hours Upon completion of the reaction, solvent is evaporated

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

実験手順: To a mixture of 5.09 g (23 mmol) of 3-aminopropyltriethoxysilane, 30 ml of 1,2-dimethoxyethane and 30 ml of 2-propanol is added 8.99 g (32.1 mmol) of the compound prepared in Example 1A. The reaction mixture is heated at a gentle reflux for 23 hours. Solvent is evaporated to afford 14.37 g of a pale yellow oil corresponding to a mixture of the title compounds. The reaction mixture is heated at a gentle reflux for 23 hours Solvent is evaporated

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

実験手順: Into a sealable, glass container were charged 50 g of γ-aminopropyl-triethoxysilane (0.226 mole) and 50 g (0.694 mole) methyl ethyl ketone. The mixture was allowed to stand one hour to permit the ketimine to form. Then 106.8 g (0.4525 mole) of γ-glicidoxypropyl-trimethoxysilane, 117.2 g of methyl ethyl ketone (1.63 mole) and 12.4 g (0.678 mole) distilled water were added to the ketimine mixture (representing a molar ratio of water per siloxane group of 0.68). The non-volatile solids content was 45 wt. % of the total coating composition, which was composed of the first component, or ketimine, and the second component (formed via partial hydrolysis of the γ-glycidoxypropyl-trimethoxysilane). The coating composition was allowed to age for about one hour, and then a sample was drawn down onto a degreased panel of polyallyl diglycol carbonate with a #22 wire wound coating rod. The coating was cured by baking at 15 hours at 80° C. The adhesion, as tested by ASTM D3359, was 100%. The scratch resistance on a Gardner Labs Scratch and Adhesion Tester was 148 g. The surface, when rubbed 100 times at 40 psi with 000 steel wool exhibited 1 or 2 scratches, but no scratches after 100 rubs at 30 psi. The usable pot life was 16-18 hours. to form

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

実験手順: This benzoxazine was prepared from 4-dodecylphenol (26.2 g, 100 mmol), 3-aminopropyltriethoxysilane (22.1 g, 100 mmol), paraformaldehyde (6.3 g, 210 mmol), and toluene (150 mL). The method to prepare this compound was the same as that used to make the previous benzoxazines. The final product was a clear, faint yellow liquid. The yield was 92%. The method to prepare this compound