丙二酸单乙酯镁

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

实验步骤: Magnesium ethyl malonate was prepared as follows: To a stirred THF solution (1 L) of monoethyl malonate (183.18 g, 1.39 mol) was added magnesium ethoxide (79.54 g, 0.70 mol) in several portions. After about 4 hours, the solvent was removed under reduced pressure and the residue was reevaporated with toluene to give magnesium ethyl malonate (190.82 g). Magnesium ethyl malonate was prepared the solvent was removed under reduced pressure the residue was reevaporated with toluene

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

实验步骤: Triethylamine (1.3 mL) and magnesium chloride (1.06 g) were added to anhydrous acetonitrile (15 mL) suspension of potassium ethylmalonate (1.58 g), and the mixture was vigorously stirred at room temperature for 18 hours under an atmosphere of argon. Next, a catalytically effective amount of N,N-dimethylaminopyridine and N,N-carbonyldiimidazole (663 mg) were added to anhydrous tetrahydrofuran (12 mL) suspension of 6-methoxy-2-(2-phenylethyl)benzimidazole-4-carboxylic acid (1.1 g) obtained in Reference Example 21, and the mixture was stirred for 2 hours under an atmosphere of argon. The reaction solution was added to the previously prepared suspension of ethyl malonate magnesium salt while cooling in an ice bath, and the mixture was stirred at room temperature for 2 hours. While cooling in an ice bath, this was diluted with water and adjusted to pH 1 with 4 N hydrochloric acid. At the same temperature, this was adjusted to pH 7 to 8 with saturated sodium bicarbonate aqueous solution and extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) and the desired fraction was concentrated to obtain the title compound as crystal (620 mg). obtained in Reference Example 21 the mixture was stirred for 2 hours under an atmosphere of argon while cooling in an ice bath the mixture was stirred at room temperature for 2 hours While cooling in an ice bath extracted with ethyl acetate The organic layer was washed with brine dried over anhydrous sodium sulfate the solvent was evaporated under a reduced pressure The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) the desired fraction was concentrated

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

实验步骤: Triethylamine (2.65 mL) and magnesium chloride (2.16 g) were added to dry acetonitrile (37.5 mL) suspension of potassium ethylmalonate (3.23 g), and the mixture was vigorously stirred at room temperature for 16 hours under in an atmosphere of argon. Next, a catalytically effective amount of N,N-dimethylaminopyridine and 1,1′-carbonyldiimidazole (1.35 g) were added to anhydrous tetrahydrofuran (30 mL) solution of 6-t-butyldimethylsilyloxy-2-(2-phenylethyl)benzimidazole-4-carboxylic acid (3.0 g) obtained in Reference Example 23, and the mixture was stirred for 1 hour under an atmosphere of argon. This was diluted to the previously prepared suspension of ethyl malonate magnesium salt while cooling in an ice bath, and the mixture was stirred at room temperature for 2 hours. This was diluted with ice water (50 mL) and, while cooling in an ice bath, adjusted to pH 1 with 4 N hydrochloric acid. While cooling in an ice bath, this was adjusted to pH 8 to 9 with saturated sodium bicarbonate aqueous solution and extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) and the desired fraction was concentrated to obtain the title compound as colorless oil (3.44 g). obtained in Reference Example 23 the mixture was stirred for 1 hour under an atmosphere of argon while cooling in an ice bath the mixture was stirred at room temperature for 2 hours while cooling in an ice bath While cooling in an ice bath extracted with ethyl acetate The organic layer was washed with brine dried over anhydrous sodium sulfate the solvent was evaporated under a reduced pressure The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) the desired fraction was concentrated

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

实验步骤: A slurry of malonate monoethyl ester magnesium salt is prepared by adding an acetone slurry of potassium malonate monoethyl ester (144 g, 846 mmoles in 350 ml of acetone) to a slurry of magnesium chloride (72 g, 756 mmoles) which has been prepared by the slow addition of acetone (250 ml) to a slurry of magnesium chloride in methylene chloride (100 ml.) The malonate salt preparation is completed by atmospheric distillation to a volume of 350 ml. is completed by atmospheric distillation to a volume of 350 ml

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

实验步骤: A slurry of malonate monoethyl ester magnesium salt is prepared by adding an acetone slurry of potassium malonate monoethyl ester (144 g, 846 mmoles in 350 ml of acetone) to a slurry of magnesium chloride (72 g, 756 mmoles) which has been prepared by the slow addition of acetone (250 ml) to a slurry of magnesium chloride in methylene chloride (100 ml.) The malonate salt preparation is completed by atmospheric distillation to a volume of 350 ml. is completed by atmospheric distillation to a volume of 350 ml

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

实验步骤: Magnesium ethyl malonate was prepared as follows: To a stirred THF solution (1 L) of monoethyl malonate (183.18 g, 1.39 mol) was added magnesium ethoxide (79.54 g, 0.70 mol) in several portions. After about 4 hours, the solvent was removed under reduced pressure and the residue was reevaporated with toluene to give magnesium ethyl malonate (190.82 g). Magnesium ethyl malonate was prepared the solvent was removed under reduced pressure the residue was reevaporated with toluene