3-溴-4-氟苯甲酰胺

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 800 g (3.6 moles) of 3-bromo-4-fluoro-benzoyl fluoride were metered into 760 g of 25% strength aqueous ammonia solution (11 moles of NH3), which had been diluted with a further 760 ml of water, at a rate such that an internal temperature of 40° to 50° C. was maintained by the weakly exothermic reaction. After stirring for a further 30 minutes, the crystalline product was isolated by filtration, washed with water and dried. 765 g (97% of theory) of 3-bromo-4-fluoro-benzoic acid amide with a melting point of 131°-133° C. were obtained. was maintained by the weakly exothermic reaction the crystalline product was isolated by filtration washed with water dried

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

实验步骤: 800 g (3.6 moles) of 3-bromo-4-fluoro-benzoyl fluoride were metered into 760 g of 25% strength aqueous ammonia solution (11 moles of NH3), which had been diluted with a further 760 ml of water, at a rate such that an internal temperature of 40° to 50° C. was maintained by the weakly exothermic reaction. After stirring for a further 30 minutes, the crystalline product was isolated by filtration, washed with water and dried. 765 g (97% of theory) of 3-bromo-4-fluoro-benzoic acid amide with a melting point of 131°-133° C. were obtained. was maintained by the weakly exothermic reaction the crystalline product was isolated by filtration washed with water dried

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

实验步骤: 765 g (3.5 moles) of 3-bromo-4-fluoro-benzoic acid amide was added, at 25° C., to 1,150 g (9.7 moles) of thionyl chloride and the mixture was heated under reflux at 85° to 90° C., while stirring, until virtually no further evolution of gas took place. The excess thionyl chloride was then distilled off and the residue was fractionated in a short column. 630 g (91% of theory) of 3-bromo-4-fluoro-benzonitrile with a boiling point of 115°-116° C./20 mm Hg were obtained. the mixture was heated under reflux at 85° to 90° C. The excess thionyl chloride was then distilled off

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 800 g (3.6 moles) of 3-bromo-4-fluoro-benzoyl fluoride were metered into 760 g of 25% strength aqueous ammonia solution (11 moles of NH3), which had been diluted with a further 760 ml of water, at a rate such that an internal temperature of 40° to 50° C. was maintained by the weakly exothermic reaction. After stirring for a further 30 minutes, the crystalline product was isolated by filtration, washed with water and dried. 765 g (97% of theory) of 3-bromo-4-fluoro-benzoic acid amide with a melting point of 131°-133° C. were obtained. was maintained by the weakly exothermic reaction the crystalline product was isolated by filtration washed with water dried

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

实验步骤: 765 g (3.5 moles) of 3-bromo-4-fluoro-benzoic acid amide was added, at 25° C., to 1,150 g (9.7 moles) of thionyl chloride and the mixture was heated under reflux at 85° to 90° C., while stirring, until virtually no further evolution of gas took place. The excess thionyl chloride was then distilled off and the residue was fractionated in a short column. 630 g (91% of theory) of 3-bromo-4-fluoro-benzonitrile with a boiling point of 115°-116° C./20 mm Hg were obtained. the mixture was heated under reflux at 85° to 90° C. The excess thionyl chloride was then distilled off