dichloro(phenyl)borane

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

実験手順: To 6.05 g of dichlorophenylborane dissolved in 40 ml of dichloromethane, at −20° C., are successively added 5.226 g of 3-methoxy-4-methylaniline dissolved in 50 ml of dichloromethane, and 13.4 ml of triethylamine dissolved in 25 ml of dichloromethane. After 30 minutes at −20° C., 5.412 g of 2,6-difluorobenzaldehyde dissolved in 60 ml of dichloromethane are introduced. After 24 hours at room temperature, the mixture is hydrolysed with water. The organic phase is dried over anhydrous sodium sulfate and concentrated. To the oil obtained, dissolved in 80 ml of diethyl ether, are added 80 ml of 2M sodium hydroxide solution and the mixture is left stirring for 18 hours. The phases are separated by settling and the organic phase is dried over anhydrous sodium sulfate and concentrated. The residue is solidified with n-pentane to give 5.069 g of the expected product. are introduced After 24 hours at room temperature The organic phase is dried over anhydrous sodium sulfate concentrated To the oil obtained the mixture is left The phases are separated the organic phase is dried over anhydrous sodium sulfate concentrated

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

実験手順: To 4.80 g (30.2 mmol) of dichloro(phenyl)borane, dissolved in 70 ml of diethyl ether, a suspension of 8.36 g (60.4 mmol) of trimethylsilylcyclopentadienyllithium in 100 ml of diethyl ether is slowly added at -78° C. The mixture is allowed to warm to room temperature in the cooling bath, and insolubles are filtered off. After concentrating the yellow filtrate to dryness in an oil-pump vacuum, 10.8 g of bis(trimethylsilylcyclopentadienyl) (phenyl)borane is obtained as a yellow viscous oil. is slowly added at -78° C are filtered off After concentrating the yellow filtrate to dryness in an oil-pump vacuum

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

実験手順: In 50 ml of diethyl ether, 5.01 g (31.5 mmol) of dichloro(phenyl)borane is cooled to -78° C. and a solution of 7.70 g (63.1 mmol) of indenyllithium in 50 ml of diethyl ether is added dropwise within one hour. After warming to room temperature, the mixture is filtered, and the slightly yellow filtrate is highly concentrated in vacuo. Gradual cooling from 0° C. to -20° C. results in the formation of 7.45 g (74%) of bis(indenyl) (phenyl)borane in the form of colorless crystals. the mixture is filtered the slightly yellow filtrate is highly concentrated in vacuo Gradual cooling from 0° C. to -20° C.

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2.230 g (7.41 mmol) of (trimethylsilylcyclopentadienyl)-trimethyltin is added 0.59 g (0.48 ml, 3.7 mmol) of dichloro-(phenyl)borane dropwise at room temperature. An intense yellow color immediately appears. The mixture is heated at 40° C. for 2 h whereupon the yellow color intensifies. This is followed by fractional distillation wherein the chlorotrimethylstannane formed can first be separated off. In the distillation, a heavy decomposition occurs from about 120° C. bath temperature to give a dark-red oil. This is followed by fractional distillation wherein the chlorotrimethylstannane formed can first be separated off In the distillation occurs from about 120° C. to give a dark-red oil

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

実験手順: N-methyl-3-methoxyanilinochlorophenylborane was prepared by adding dichlorophenylborane (100 mmol) to a solution of N-methy-3-methoxyaniline (100 mmol) in 1,2-dichloroethane (100 mL) at 0° C. The resulting mixture was refluxed for 2 h under a rapid stream of nitrogen to remove the HCl formed. The mixture was cooled to give a 0.8 M cloudy solution of the title compound which could be stored at 0°C. for more than 6 weeks without deterioration. N-methyl-3-methoxyanilinochlorophenylborane was prepared The resulting mixture was refluxed for 2 h under a rapid stream of nitrogen to remove the HCl formed The mixture was cooled

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

実験手順: To 6.05 g of dichlorophenylborane dissolved in 40 ml of dichloromethane, at −20° C., are successively added 5.226 g of 3-methoxy-4-methylaniline dissolved in 50 ml of dichloromethane, and 13.4 ml of triethylamine dissolved in 25 ml of dichloromethane. After 30 minutes at −20° C., 5.412 g of 2,6-difluorobenzaldehyde dissolved in 60 ml of dichloromethane are introduced. After 24 hours at room temperature, the mixture is hydrolysed with water. The organic phase is dried over anhydrous sodium sulfate and concentrated. To the oil obtained, dissolved in 80 ml of diethyl ether, are added 80 ml of 2M sodium hydroxide solution and the mixture is left stirring for 18 hours. The phases are separated by settling and the organic phase is dried over anhydrous sodium sulfate and concentrated. The residue is solidified with n-pentane to give 5.069 g of the expected product. are introduced After 24 hours at room temperature The organic phase is dried over anhydrous sodium sulfate concentrated To the oil obtained the mixture is left The phases are separated the organic phase is dried over anhydrous sodium sulfate concentrated