2-溴-1,3-二氯-5-氟苯

反应条件: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Diethyl malonate (0.49 mol) is added to a mixture of sodium hydride (0.51 mol) and 1,4-dioxane (140 ml) at 55 to 60° C. within 2 hours. The mixture is stirred for 10 minutes at 55° C. and copper(I) bromide (0.05 mol) is added. After 15 minutes a mixture of 1-bromo-2,6-dichloro-4-fluoro-benzene (0.25 mol) and 1,4-dioxane (10 ml) is added. The reaction mixture is heated at 100° C. for 15 hours and cooled to 15° C. Hydrochloric acid (12N, 35 ml) is added slowly at 15 to 20° C. The precipitate is filtered off. The filtrate is extracted with diethylether. The organic phase is separated, dried with anhydrous sodium sulphate and filtered. The filtrate is evaporated under reduced pressure to yield 44 g of the product as yellow crystals having a melting point of 170° C. is added The reaction mixture is heated at 100° C. for 15 hours cooled to 15° C The precipitate is filtered off The filtrate is extracted with diethylether The organic phase is separated dried with anhydrous sodium sulphate filtered The filtrate is evaporated under reduced pressure

反应条件: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Diethyl malonate (0.49 mol) is added to a mixture of sodium hydride (0.51 mol) and 1,4-dioxane (140 ml) at 55 to 60° C. within 2 hours. The mixture is stirred for 10 minutes at 55° C. and copper(I) bromide (0.05 mol) is added. After 15 minutes a mixture of 1-bromo-2,6-dichloro-4-fluoro-benzene (0.25 mol) and 1,4-dioxane (10 ml) is added. The reaction mixture is heated at 100° C. for 15 hours and cooled to 15° C. Hydrochloric acid (12N, 35 ml) is added slowly at 15 to 20° C. The precipitate is filtered off. The filtrate is extracted with diethylether. The organic phase is separated, dried with anhydrous sodium sulphate and filtered. The filtrate is evaporated under reduced pressure to yield 44 g of the product as yellow crystals having a melting point of 170° C. is added The reaction mixture is heated at 100° C. for 15 hours cooled to 15° C The precipitate is filtered off The filtrate is extracted with diethylether The organic phase is separated dried with anhydrous sodium sulphate filtered The filtrate is evaporated under reduced pressure

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

实验步骤: Bromine (0.6 mol) is added to a mixture of 1,3-dichloro-5-fluorobenzene (0.6 mol) and ferrous powder within 2 hours. The brown reaction mixture is stirred 16 hours at room temperature and subsequently washed with dichloromethane and water. The organic layer is separated, washed with sodium hydrogen carbonate solution and dried with anhydrous sodium sulphate. The solvent is evaporated under reduced pressure. The raw product is recrystallized in ethanol to yield 61 g of the product as a white powder having a melting point of 83° C. subsequently washed with dichloromethane and water The organic layer is separated washed with sodium hydrogen carbonate solution dried with anhydrous sodium sulphate The solvent is evaporated under reduced pressure The raw product is recrystallized in ethanol

反应条件: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Diethyl malonate (0.49 mol) is added to a mixture of sodium hydride (0.51 mol) and 1,4-dioxane (140 ml) at 55 to 60° C. within 2 hours. The mixture is stirred for 10 minutes at 55° C. and copper(I) bromide (0.05 mol) is added. After 15 minutes a mixture of 1-bromo-2,6-dichloro-4-fluoro-benzene (0.25 mol) and 1,4-dioxane (10 ml) is added. The reaction mixture is heated at 100° C. for 15 hours and cooled to 15° C. Hydrochloric acid (12N, 35 ml) is added slowly at 15 to 20° C. The precipitate is filtered off. The filtrate is extracted with diethylether. The organic phase is separated, dried with anhydrous sodium sulphate and filtered. The filtrate is evaporated under reduced pressure to yield 44 g of the product as yellow crystals having a melting point of 170° C. is added The reaction mixture is heated at 100° C. for 15 hours cooled to 15° C The precipitate is filtered off The filtrate is extracted with diethylether The organic phase is separated dried with anhydrous sodium sulphate filtered The filtrate is evaporated under reduced pressure

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

实验步骤: Bromine (0.6 mol) is added to a mixture of 1,3-dichloro-5-fluorobenzene (0.6 mol) and ferrous powder within 2 hours. The brown reaction mixture is stirred 16 hours at room temperature and subsequently washed with dichloromethane and water. The organic layer is separated, washed with sodium hydrogen carbonate solution and dried with anhydrous sodium sulphate. The solvent is evaporated under reduced pressure. The raw product is recrystallized in ethanol to yield 61 g of the product as a white powder having a melting point of 83° C. subsequently washed with dichloromethane and water The organic layer is separated washed with sodium hydrogen carbonate solution dried with anhydrous sodium sulphate The solvent is evaporated under reduced pressure The raw product is recrystallized in ethanol