丁烷-1-olate;titanium(4+)

反应条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The reaction apparatus consisted of a heated enameled vessel of two cubic meters capacity, equipped with three feed tubes, a stirrer, and a glass condenser operated with water and connected to a 4 square meter Hastelloy C brine cooler (-45° C.). 670 liters of hexane were placed in it and refluxed. The temperature below the water condenser amounted to 69° C. Over a period of 2 hours 380 kg of titanium chloride (2 kmol) and 444 kg of n-butanol (6 kmol) were put in at such a rate that the molar ratio of titanium chloride to n-butanol amounted always to about 1:3. Immediately at the start of the addition a vigorous evolution of hydrogen chloride began. The temperature below the water condenser dropped to 60° C. and rose toward the end of the reaction back to 64° C. After the reaction another 155.4 kg of n-butanol (2.1 kmol) was added with stirring. A sample had a chlorine content of 11.6%. This meant that 47.5% of the chlorine present had been removed in the form of hydrogen chloride. After cooling to about 30° C., the mixture was first diluted with 200 liters of hexane, and then ammonia was fed through the third feed tube for a period of 2 hours. The suspension obtained was centrifuged to separate the precipitated ammonium chloride. First the hexane was distilled out of the filtrate; then, at a vacuum of less than 1 mbar and at a head temperature of about 155° C., the butyl titanate was purified by distillation. 619 kg of butyl titanate was obtained. The reaction apparatus consisted of a heated enameled vessel of two cubic meters capacity equipped with three feed tubes, a stirrer, and a glass condenser refluxed amounted to 69° C rose toward the end of the reaction back to 64° C was added present had been removed in the form of hydrogen chloride the mixture was first diluted with 200 liters of hexane The suspension obtained to separate the precipitated ammonium chloride First the hexane was distilled out of the filtrate then, at a vacuum of less than 1 mbar and at a head temperature of about 155° C., the butyl titanate was purified by distillation

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 152 g (1 mol) of 2-(ethylhydroxyphosphinyl)acetic acid (produced as in Example 11) and 170 g of titanium tetrabutoxide are refluxed in 500 ml of toluene for 40 hours. The resulting butanol is distilled off from time to time with proportions of toluene. The solution formed is subsequently freed of solvent to leave 167 g (96% of theory) of 2-(ethylhydroxyphosphinyl)acetic acid titanium salt. The resulting butanol is distilled off from time to time with proportions of toluene The solution formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 180 g (1 mol) of 3-(ethylhydroxyphosphinyl)-2-methylpropionic acid (produced as in Example 17) and 170 g of titanium tetrabutoxide are refluxed in 500 ml of toluene for 40 hours. The resulting butanol is distilled off from time to time with proportions of toluene. The solution formed is subsequently freed of solvent to leave 184 g (91% of theory) of 3-(ethylhydroxyphosphinyl)-2-methylpropionic acid titanium salt. The resulting butanol is distilled off from time to time with proportions of toluene The solution formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 152 g (1 mol) of 2-(ethylhydroxyphosphinyl)acetic acid (produced as in Example 10) and 170 g of titanium tetrabutoxide are refluxed in 500 ml of toluene for 40 hours. The resulting butanol is distilled off from time to time with proportions of toluene. The solution formed is subsequently freed of solvent to leave 167 g (96% of theory) of 2-(ethylhydroxyphosphinyl)acetic acid titanium salt. The resulting butanol is distilled off from time to time with proportions of toluene The solution formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 152 g (1 mol) of 2-(ethylhydroxyphosphinyl)acetic acid (produced as in Example 10) and 170 g of titanium tetrabutoxide are refluxed in 500 ml of toluene for 40 hours. The resulting butanol is distilled off from time to time with proportions of toluene. The solution formed is subsequently freed of solvent to leave 167 g (96% of theory) of 2-(ethylhydroxyphosphinyl)acetic acid titanium salt. The resulting butanol is distilled off from time to time with proportions of toluene The solution formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 138 g (1 mol) of ethyl(2-hydroxyethyl)phosphinic acid (produced as in Example 7) and 85 g of titanium tetrabutoxide are refluxed in 500 ml of toluene for 40 hours. The resulting butanol is distilled off from time to time with proportions of toluene. The solution formed is subsequently freed of solvent to leave 136 g (91% of theory) of ethyl(2-hydroxyethyl)phosphinic acid titanium salt. The resulting butanol is distilled off from time to time with proportions of toluene The solution formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 138 g (1 mol) of ethyl(2-hydroxyethyl)phosphinic acid (produced as in Example 7) and 85 g of titanium tetrabutoxide are refluxed in 500 ml of toluene for 40 hours. The resulting butanol is distilled off from time to time with proportions of toluene. The solution formed is subsequently freed of solvent to leave 136 g (91% of theory) of ethyl(2-hydroxyethyl)phosphinic acid titanium salt. The resulting butanol is distilled off from time to time with proportions of toluene The solution formed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Pinacol (130 g) was added to BOH solution (500 g) of a titanium tetrabutoxide tetramer (243 g) and agitated at room temperature for 30 minutes. After the solution was concentrated under reduced pressure at 40° C., it was heated to 60° C. and heating was continued under reduced pressure to generate no distillate. Then, PGMEA (1,200 g) was added thereto and heated under reduced pressure at 50° C. until no BOH was distilled to obtain a PGMEA solution of a titanium-containing compound [B-IV] (1,000 g) (compound concentration: 22%). The molecular weight (Mw) of the compound measured in terms of polystyrene was 1,150. After the solution was concentrated under reduced pressure at 40° C. it was heated to 60° C. heating Then, PGMEA (1,200 g) was added heated under reduced pressure at 50° C. until no BOH was distilled

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1-butanol (BOH) solution (500 g) of deionized water (27 g) was agitated with BOH solution (500 g) of a titanium tetrabutoxide (340 g) and dropped at room temperature for 2 hours. 3-methyl-1,3-hexanediol (132 g) was added to a solution obtained and agitated at room temperature for 30 minutes. After the solution was concentrated under reduced pressure at 40° C., it was heated to 60° C. and heating was continued under reduced pressure to generate no distillate. Then, PGMEA (1,200 g) was added thereto and heated under reduced pressure at 50° C. until no BOH was distilled to obtain a PGMEA solution of a titanium-containing compound [B-III] (1,000 g) (compound concentration: 22%). The molecular weight (Mw) of the compound measured in terms of polystyrene was 1,250. dropped at room temperature for 2 hours obtained After the solution was concentrated under reduced pressure at 40° C. it was heated to 60° C. heating Then, PGMEA (1,200 g) was added heated under reduced pressure at 50° C. until no BOH was distilled

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1-butanol (BOH) solution (500 g) of deionized water (27 g) was agitated with BOH solution (500 g) of a titanium tetrabutoxide (340 g) and dropped at room temperature for 2 hours. 3-methyl-1,3-hexanediol (132 g) was added to a solution obtained and agitated at room temperature for 30 minutes. After the solution was concentrated under reduced pressure at 40° C., it was heated to 60° C. and heating was continued under reduced pressure to generate no distillate. Then, PGMEA (1,200 g) was added thereto and heated under reduced pressure at 50° C. until no BOH was distilled to obtain a PGMEA solution of a titanium-containing compound [B-III] (1,000 g) (compound concentration: 22%). The molecular weight (Mw) of the compound measured in terms of polystyrene was 1,250. dropped at room temperature for 2 hours obtained After the solution was concentrated under reduced pressure at 40° C. it was heated to 60° C. heating Then, PGMEA (1,200 g) was added heated under reduced pressure at 50° C. until no BOH was distilled

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Pinacol (130 g) was added to BOH solution (500 g) of a commercially available titanium tetrabutoxide tetramer (243 g) and agitated at room temperature for 30 minutes. After the solution was concentrated under reduced pressure at 40° C., it was heated to 60° C. and heating was continued under reduced pressure to generate no distillate. Then, PGMEA (1,200 g) was added thereto and heated under reduced pressure at 50° C. until no BOH was distilled to obtain a PGMEA solution of a titanium-containing compound [A-IV] (1,000 g) (compound concentration: 22%). The molecular weight (Mw) of the compound measured in terms of polystyrene was 1,150. After the solution was concentrated under reduced pressure at 40° C. it was heated to 60° C. heating Then, PGMEA (1,200 g) was added heated under reduced pressure at 50° C. until no BOH was distilled

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1-butanol (BOH) solution (500 g) of deionized water (27 g) was agitated with BOH solution (500 g) of a titanium tetrabutoxide (340 g) and dropped at room temperature for 2 hours. 3-methyl-1,3-hexanediol (132 g) was added to a solution obtained and agitated at room temperature for 30 minutes. After the solution was concentrated under reduced pressure at 40° C., it was heated to 60° C. and heating was continued under reduced pressure to generate no distillate. Then, propylene glycol methyl ether acetate (PGMEA) (1,200 g) was added thereto and heated under reduced pressure at 50° C. until no BOH was distilled to obtain a PGMEA solution of a titanium-containing compound [A-III] (1,000 g) (compound concentration: 22%). The molecular weight (Mw) of the compound measured in terms of polystyrene was 1,250. dropped at room temperature for 2 hours obtained After the solution was concentrated under reduced pressure at 40° C. it was heated to 60° C. heating Then, propylene glycol methyl ether acetate (PGMEA) (1,200 g) was added heated under reduced pressure at 50° C. until no BOH was distilled