瑞巴派特杂质14

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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: An amount of 123.8 g (795.5 mmol) of 4-chlorobenzenecarboxamide and 101.0 g (795.5 mmol) of 1,3-dichloroacetone were stirred at 135° C. for an hour. A melt was formed. The batch was subsequently cooled to RT with stirring, and at this temperature it was admixed cautiously with 200 ml of concentrated sulfuric acid and stirred for 30 minutes. The resulting suspension was poured into ice-water and stirred for a further 30 minutes. The precipitate formed was then isolated by suction filtration, washed with water and purified by flash chromatography on silica gel (eluent: dichloromethane). The solvent was removed on a rotary evaporator and the residue was dried under reduced pressure. This gave 95.5 g (53% of theory) of the target compound. A melt was formed stirred for 30 minutes stirred for a further 30 minutes The precipitate formed was then isolated by suction filtration washed with water purified by flash chromatography on silica gel (eluent: dichloromethane) The solvent was removed on a rotary evaporator the residue was dried under reduced pressure