锌;2,2-二甲基丙酸酯

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

实验步骤: The 3-(trifluormethyl)phenylzinc pivalate (1d) product can be stored under inert gas atmosphere at ambient temperature for one week without any loss of activity (entry 1, Table 1 below). After 5 minutes of storage in air, 95% of active zinc species could be determined by titration (Table 1, entry 2). After 15 minutes, the activity is reduced to 58% (Table 1, entry 3) and after 30 and 45 minutes, activities of 43% and 40% are obtained (Table 1, entries 4-5). After storage on air for 60 minutes, active zinc species cannot be detected (Table 1, entry 6). after 30 and 45 minutes, activities of 43% and 40% are obtained (Table 1, entries 4-5) After storage on air for 60 minutes

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2LiCl (2a prepared above; 2.64 g, 7.50 mmol) is placed in a 25 mL Schlenk-flask, dried for 5 min at 400° C. (heat gun) in high vacuum and then dissolved in dry THF (10.0 mL). 1-Bromo-3-(trifluoromethyl)benzene (3d; 1.13 g, 5.00 mmol) and magnesium-turnings (304 mg, 12.5 mmol) are added and the mixture was stirred for 2 h at 25° C. The solution is cannulated to a dry and argon-flushed 50 mL Schlenk-tube via syringe filter and the solvent is removed in vacuo. 3-(Trifluoromethyl)phenylzinc pivalate (1d) is obtained as a grey solid (3.72 g). is placed in a 25 mL Schlenk-flask dried for 5 min at 400° C. (heat gun) in high vacuum dissolved in dry THF (10.0 mL) a dry argon-flushed 50 mL Schlenk-tube via syringe filter the solvent is removed in vacuo

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2LiCl (2a prepared above; 2.64 g, 7.50 mmol) is placed in a 25 mL Schlenk-flask, dried for 5 min at 400° C. (heat gun) in high vacuum and then dissolved in dry THF (10.0 mL). 1-Bromo-3-(trifluoromethyl)benzene (3d; 1.13 g, 5.00 mmol) and magnesium-turnings (304 mg, 12.5 mmol) are added and the mixture was stirred for 2 h at 25° C. The solution is cannulated to a dry and argon-flushed 50 mL Schlenk-tube via syringe filter and the solvent is removed in vacuo. 3-(Trifluoromethyl)phenylzinc pivalate (1d) is obtained as a grey solid (3.72 g). is placed in a 25 mL Schlenk-flask dried for 5 min at 400° C. (heat gun) in high vacuum dissolved in dry THF (10.0 mL) a dry argon-flushed 50 mL Schlenk-tube via syringe filter the solvent is removed in vacuo

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Pivalic acid (20.4 g, 22.6 mL, 200 mmol) is placed in a dry and argon-flushed 500 mL Schlenk-flask equipped with a magnetic stirring bar and a septum, and the pivalic acid is dissolved in dry THF (100 mL). The solution is cooled to 0° C. and methyllithium (135 mL, 1.63 M in diethyl ether, 220 mmol) is added dropwise. After the evolution of methane gas has stopped, ZnCl2 in THF (100 mL, 1.0 M, 100 mmol) is added and the mixture is stirred for 2 h at 25° C. The solvent is removed in vacuo and zinc pivalate.2LiCl (2a) is obtained as a colourless solid in quantitative yield. a dry argon-flushed 500 mL Schlenk-flask equipped with a magnetic stirring bar a septum, and the pivalic acid is dissolved in dry THF (100 mL) The solvent is removed in vacuo and zinc pivalate

反应条件: temp:4.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 250 ml of water, warmed to 60°-70° C., was added 56.1 gm (0.55 mole) of pivalic acid (trimethylacetic acid). Then 31.25 gm (0.25 mole) of zinc carbonate was added portionwise over a period of 10 to 15 minutes and then the temperature was raised to 96°-98° C. After agitating the reaction mixture for 1 hour, the mixture was cooled to 4° C. with an ice bath for 30 minutes and the suspension filtered. The filter cake was washed once with 75 ml cold water and 3×50 ml cold acetone. The resulting product was dried at 60° C. for 16 hours in a draft oven to yield 58 gm (87%) of zinc pivaloate. the temperature was raised to 96°-98° C the suspension filtered The filter cake was washed once with 75 ml cold water and 3×50 ml cold acetone The resulting product was dried at 60° C. for 16 hours in a draft oven

反应条件: temp:4.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 250 ml of water, warmed to 60°-70° C., was added 56.1 gm (0.55 mole) of pivalic acid (trimethylacetic acid). Then 31.25 gm (0.25 mole) of zinc carbonate was added portionwise over a period of 10 to 15 minutes and then the temperature was raised to 96°-98° C. After agitating the reaction mixture for 1 hour, the mixture was cooled to 4° C. with an ice bath for 30 minutes and the suspension filtered. The filter cake was washed once with 75 ml cold water and 3×50 ml cold acetone. The resulting product was dried at 60° C. for 16 hours in a draft oven to yield 58 gm (87%) of zinc pivaloate. the temperature was raised to 96°-98° C the suspension filtered The filter cake was washed once with 75 ml cold water and 3×50 ml cold acetone The resulting product was dried at 60° C. for 16 hours in a draft oven

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

实验步骤: The 3-(trifluormethyl)phenylzinc pivalate (1d) product can be stored under inert gas atmosphere at ambient temperature for one week without any loss of activity (entry 1, Table 1 below). After 5 minutes of storage in air, 95% of active zinc species could be determined by titration (Table 1, entry 2). After 15 minutes, the activity is reduced to 58% (Table 1, entry 3) and after 30 and 45 minutes, activities of 43% and 40% are obtained (Table 1, entries 4-5). After storage on air for 60 minutes, active zinc species cannot be detected (Table 1, entry 6). after 30 and 45 minutes, activities of 43% and 40% are obtained (Table 1, entries 4-5) After storage on air for 60 minutes

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2LiCl (2a prepared above; 2.64 g, 7.50 mmol) is placed in a 25 mL Schlenk-flask, dried for 5 min at 400° C. (heat gun) in high vacuum and then dissolved in dry THF (10.0 mL). 1-Bromo-3-(trifluoromethyl)benzene (3d; 1.13 g, 5.00 mmol) and magnesium-turnings (304 mg, 12.5 mmol) are added and the mixture was stirred for 2 h at 25° C. The solution is cannulated to a dry and argon-flushed 50 mL Schlenk-tube via syringe filter and the solvent is removed in vacuo. 3-(Trifluoromethyl)phenylzinc pivalate (1d) is obtained as a grey solid (3.72 g). is placed in a 25 mL Schlenk-flask dried for 5 min at 400° C. (heat gun) in high vacuum dissolved in dry THF (10.0 mL) a dry argon-flushed 50 mL Schlenk-tube via syringe filter the solvent is removed in vacuo

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Pivalic acid (20.4 g, 22.6 mL, 200 mmol) is placed in a dry and argon-flushed 500 mL Schlenk-flask equipped with a magnetic stirring bar and a septum, and the pivalic acid is dissolved in dry THF (100 mL). The solution is cooled to 0° C. and methyllithium (135 mL, 1.63 M in diethyl ether, 220 mmol) is added dropwise. After the evolution of methane gas has stopped, ZnCl2 in THF (100 mL, 1.0 M, 100 mmol) is added and the mixture is stirred for 2 h at 25° C. The solvent is removed in vacuo and zinc pivalate.2LiCl (2a) is obtained as a colourless solid in quantitative yield. a dry argon-flushed 500 mL Schlenk-flask equipped with a magnetic stirring bar a septum, and the pivalic acid is dissolved in dry THF (100 mL) The solvent is removed in vacuo and zinc pivalate