difluoromethoxybenzene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: 0.5 g of potassium chloride and 10 g of difluoromethoxybenzene in 100 ml of 1,3-bistrifluoromethylbenzene were introduced as the initial charge, and chlorine was then introduced at 100° C. with UV irradiation. In the course of an hour, another 20 g of difluoromethoxybenzene were metered in. After chlorine uptake was complete, the reaction mixture was purged with nitrogen and subsequently distilled. 35.5 g of chlorodifluoromethoxybenzene were isolated (boiling point 144° C., refractive index nD20 1.4479). initial charge In the course of an hour the reaction mixture was purged with nitrogen subsequently distilled

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

実験手順: A solution of 3-(difluoromethoxy)benzene (3.0 g) and triisopropoxyborane (2.78 g) in tetrahydrofuran (15 ml) was cooled to −78° C. under argon atmosphere, and thereto was added a solution of n-butyl lithium (1.59 M hexane solution, 9.3 ml). The mixture was stirred at same temperature for 10 minutes, warmed, and further stirred at room temperature overnight. Thereto was added 3N aqueous hydrochloric acid solution (10 ml), and the mixture was stirred at room temperature for 5 minutes. The mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was crystallized from hexane to give 3-difluoromethoxybenzene-boronic acid (1.6 g) as colorless crystals. warmed further stirred at room temperature overnight the mixture was stirred at room temperature for 5 minutes The mixture was extracted with ethyl acetate The extract was washed with brine dried over sodium sulfate The solvent was evaporated under reduced pressure The residue was crystallized from hexane

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

実験手順: 0.5 g of potassium chloride and 10 g of difluoromethoxybenzene in 100 ml of 1,3-bistrifluoromethylbenzene were introduced as the initial charge, and chlorine was then introduced at 100° C. with UV irradiation. In the course of an hour, another 20 g of difluoromethoxybenzene were metered in. After chlorine uptake was complete, the reaction mixture was purged with nitrogen and subsequently distilled. 35.5 g of chlorodifluoromethoxybenzene were isolated (boiling point 144° C., refractive index nD20 1.4479). initial charge In the course of an hour the reaction mixture was purged with nitrogen subsequently distilled

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

実験手順: 0.5 g of potassium chloride and 10 g of difluoromethoxybenzene in 100 ml of 1,3-bistrifluoromethylbenzene were introduced as the initial charge, and chlorine was then introduced at 100° C. with UV irradiation. In the course of an hour, another 20 g of difluoromethoxybenzene were metered in. After chlorine uptake was complete, the reaction mixture was purged with nitrogen and subsequently distilled. 35.5 g of chlorodifluoromethoxybenzene were isolated (boiling point 144° C., refractive index nD20 1.4479). initial charge In the course of an hour the reaction mixture was purged with nitrogen subsequently distilled

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

実験手順: A solution of 3-(difluoromethoxy)benzene (3.0 g) and triisopropoxyborane (2.78 g) in tetrahydrofuran (15 ml) was cooled to −78° C. under argon atmosphere, and thereto was added a solution of n-butyl lithium (1.59 M hexane solution, 9.3 ml). The mixture was stirred at same temperature for 10 minutes, warmed, and further stirred at room temperature overnight. Thereto was added 3N aqueous hydrochloric acid solution (10 ml), and the mixture was stirred at room temperature for 5 minutes. The mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was crystallized from hexane to give 3-difluoromethoxybenzeneboronic acid (1.6 g) as colorless crystals. warmed further stirred at room temperature overnight the mixture was stirred at room temperature for 5 minutes The mixture was extracted with ethyl acetate The extract was washed with brine dried over sodium sulfate The solvent was evaporated under reduced pressure The residue was crystallized from hexane

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

実験手順: A solution of 3-(difluoromethoxy)benzene (3.0 g) and triisopropoxyborane (2.78 g) in tetrahydrofuran (15 ml) was cooled to −78° C. under argon atmosphere, and thereto was added a solution of n-butyl lithium (1.59 M hexane solution, 9.3 ml). The mixture was stirred at same temperature for 10 minutes, warmed, and further stirred at room temperature overnight. Thereto was added 3N aqueous hydrochloric acid solution (10 ml), and the mixture was stirred at room temperature for 5 minutes. The mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was crystallized from hexane to give 3-difluoromethoxybenzeneboronic acid (1.6 g) as colorless crystals. warmed further stirred at room temperature overnight the mixture was stirred at room temperature for 5 minutes The mixture was extracted with ethyl acetate The extract was washed with brine dried over sodium sulfate The solvent was evaporated under reduced pressure The residue was crystallized from hexane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir: