Gallium

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

実験手順: A mixture of 0.1 g of 6-acetyl-3-(3,4-dimethoxybenzyl)-1-(tetrahydro-2H-pyran-4-yl)-quinazoline-2,4(1H,3H)-dione, 0.057 g of potassium iodide, 0.01 g of lithium chloride, 0.019 g of gallium and 0.065 g of trimethylsilylpropargyl bromide in 1 ml of THF is refluxed for 2 hours and then left for 2 days at room temperature. The reaction mixture is filtered through Celite and evaporated under reduced pressure. The residue is chromatographed on silica gel, eluting with a DCM/EtOAc mixture from (70/30, v/v) to give 0.112 g of the expected product. is refluxed for 2 hours The reaction mixture is filtered through Celite evaporated under reduced pressure The residue is chromatographed on silica gel eluting with a DCM/EtOAc mixture from (70/30, v/v)

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

実験手順: The 3-hydroxy-3-alkylated acetylenic compounds of this invention are prepared by employing the appropriately alkylated alkynyl boron, alkynyl gallium or alkynyl aluminum reactant. For example, treatment of methyl 3-hydroxy-5-oxocyclopent-1-eneheptanoate with tri(3methyl-3-[tetrahydropyran-2-yl]oxy-1-octynyl) aluminum, gallium or boron affords the epimeric methyl 3-hydroxy-2-(3-methyl-3-[tetrahydropyran-2-yl]oxy-1-octynyl)-5-oxocyclopentaneheptanoate. Typically, that compound may be hydrolyzed with a hydrolyzing agent such as hydrolytic acid, e.g. aqueous acetic acid, to yield the instant methyl 3-hydroxy-2-(3-hydroxy-3-methyl-1-octynyl)-5-oxocyclopentaneheptanoate.

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

実験手順: The 3-hydroxy-3-alkylated acetylenic compounds of this invention are prepared by employing the appropriately alkylated alkynyl boron, alkynyl gallium or alkynyl aluminum reactant. For example, treatment of methyl 3-hydroxy-5-oxocyclopent-1-eneheptanoate with tri(3methyl-3-[tetrahydropyran-2-yl]oxy-1-octynyl) aluminum, gallium or boron affords the epimeric methyl 3-hydroxy-2-(3-methyl-3-[tetrahydropyran-2-yl]oxy-1-octynyl)-5-oxocyclopentaneheptanoate. Typically, that compound may be hydrolyzed with a hydrolyzing agent such as hydrolytic acid, e.g. aqueous acetic acid, to yield the instant methyl 3-hydroxy-2-(3-hydroxy-3-methyl-1-octynyl)-5-oxocyclopentaneheptanoate.

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To gallium ethoxide (1.06 gram, 0.00517 mol, AlfaAesar 41907) was added methoxyethoxyacetic anhydride (4.16 gram, 0.0167 mol, made by the reaction of methoxyethoxyacetic acid and acetic anhydride). The contents of the reaction mixture were heated to 60° C. for 18 hours to give a viscous liquid mixture of the product and the by-product the ethylester of methoxyethoxyacetic acid. The mixture was soluble and stable in water and in dilute aqueous hydrochloric acid. The product mixture containing the ester and gallium salt left a 6.09% ceramic oxide residue as measured by TGA in air. IR(thin film) 2984, 2931, 2894, 1753, 1603, 1457, 1204, 1145, 1101 cm−1. to give a viscous liquid mixture of the product

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

実験手順: Sol-gel libraries were deposited on silicon wafer substrates. Stock solutions of yttrium isopropoxide, aluminum isopropoxide, gadolinium isopropoxide and gallium isopropoxide were prepared in 2-methoxyethanol (0.25 M) refluxing under Argon for 8 hours. To each of the four stock solutions of yttrium, gadolinium, aluminum and gallium in methoxyethanol (0.25 M), 1 equivalent of 2,4-pentandione was added with stirring, followed by the addition of anhydrous ethylene glycol (15% v/v). The yttrium and gadolinium solutions contained Ce(NO)3.6H2O at 1.0 mol % as the dopant source. refluxing under Argon for 8 hours

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

実験手順: 4.1 g of gallium sulphate hydrate (the H2O/Ga2 (SO4)3 molar ratio is close to 25) are dissolved in 3.7 g of distilled water. The sulphate is obtained by dissolving gallium (Grade 1 from Johnson Matthey) in hot concentrated H2SO4, in excess, taking up the suspension obtained in ethanol at a concentration of 60% in water at normal temperature, reprecipitation, in this cooled solution, of gallium sulphate hydrate by adding ether followed by filtration and controlled drying. 1.15 g of 85% phosphoric acid (Prolabo) are added with stirring followed by 0.25 g of 40% hydrofluoric acid (Fluka) and, lastly, 4.55 g of di-n-propylamine (Fluka), abbreviated to DPA in what follows. Stirring is continued for approximately 15 minutes. The pH is then 6.

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

実験手順: 4.1 g of gallium sulphate hydrate (the H2O/Ga2 (SO4)3 molar ratio is close to 25) are dissolved in 3.7 g of distilled water. The sulphate is obtained by dissolving gallium (Grade 1 from Johnson Matthey) in hot concentrated H2SO4, in excess, taking up the suspension obtained in ethanol at a concentration of 60% in water at normal temperature, reprecipitation, in this cooled solution, of gallium sulphate hydrate by adding ether followed by filtration and controlled drying. 1.15 g of 85% phosphoric acid (Prolabo) are added with stirring followed by 0.25 g of 40% hydrofluoric acid (Fluka) and, lastly, 4.55 g of di-n-propylamine (Fluka), abbreviated to DPA in what follows. Stirring is continued for approximately 15 minutes. The pH is then 6.

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To gallium ethoxide (1.06 gram, 0.00517 mol, AlfaAesar 41907) was added methoxyethoxyacetic anhydride (4.16 gram, 0.0167 mol, made by the reaction of methoxyethoxyacetic acid and acetic anhydride). The contents of the reaction mixture were heated to 60° C. for 18 hours to give a viscous liquid mixture of the product and the by-product the ethylester of methoxyethoxyacetic acid. The mixture was soluble and stable in water and in dilute aqueous hydrochloric acid. The product mixture containing the ester and gallium salt left a 6.09% ceramic oxide residue as measured by TGA in air. IR (thin film) 2984, 2931, 2894, 1753,1603, 1457, 1204, 1145, 1101 cm−1. to give a viscous liquid mixture of the product

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

実験手順: Other 1:1 gallium complexes with polyalcohols can be prepared in a similar fashion by substituting another polyalcohol ligand for the xylitol ligand in this procedure. Similarly, the 2:1 gallium complex with a polyalcohol can be prepared by adding 0.25 mole, instead of 0.5 mole, of polyalcohol ligand to the heated anhydrous gallium isopropoxide solution in this procedure. by adding 0.25 mole

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

実験手順: Sol-gel libraries were deposited on silicon wafer substrates. Stock solutions of yttrium isopropoxide, aluminum isopropoxide, gadolinium isopropoxide and gallium isopropoxide were prepared in 2-methoxyethanol (0.25 M) refluxing under Argon for 8 hours. To each of the four stock solutions of yttrium, gadolinium, aluminum and gallium in methoxyethanol (0.25 M), 1 equivalent of 2,4-pentandione was added with stirring, followed by the addition of anhydrous ethylene glycol (15% v/v). The yttrium and gadolinium solutions contained Ce(NO)3.6H2O at 1.0 mol % as the dopant source. refluxing under Argon for 8 hours

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

実験手順: The present invention provides a process for producing hydroxygallium phthalocyanine crystals, which process comprises reacting a gallium compound with an excess of a compound forming a phthalocyanine ring to prepare gallium phthalocyanine, subjecting the resulting gallium. phthalocyanine to acid pasting to obtain a hydroxygallium phthalocyanine crystal having intense diffraction peaks at Bragg angles (2θ±0.2°) of 6.9°, 13.2° to 14.2°, 16.5°, and 26.4° or of 7.0°, 13.4°, 16.6°, 26.0°, and 26.7° in Cukα characteristic X-ray diffractometry, and transforming the resulting crystal by a solvent treatment into hydroxygallium phthalocyanine crystals having intense diffraction peaks at Bragg angles (2θ±0.2°) of 7.5°, 9.9°, 12.5°, 16.3°, 18.6°, 25.1°, and 28.3° in Cukα characteristic X-ray diffractometry. forming a phthalocyanine ring

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

実験手順: A solution of gallium nitrate was prepared as follows: 57.45 parts of gallium were dissolved in 400 ml conc. nitric acid. The mixture was heated until brown fumes appeared, when the heat was removed and the container covered. After standing overnight, the resultant green solution was alternately heated and cooled until it turned yellow, and then clear. Deionized water was added to form 1000 ml of solution. The mixture was heated until brown fumes when the heat was removed the resultant green solution was alternately heated cooled until it Deionized water was added