2,5-dibromobenzoyl chloride

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: Under a blanket of nitrogen, 2,5-dibromobenzoyl chloride (57.43 g, 0.11925 mol) was added to a solution of 4-octyloxybenzoic acid hydrazide (50.88 g, 0.1925 mol) and triethylamine (27 mL, 19.48 g, 0.1925 mol) in 800 mL of methylene chloride. The reaction mixture was stirred for 5 hours at room temperature. The precipitated solid was filtered off and re-crystallized from hot DMF/water gave 79.38 g (78% yield) 2,5-dibromo-N′-[4-(octyloxy)benzoyl]benzohydrazide. The precipitated solid was filtered off re-crystallized from hot DMF/water

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

実験手順: Into a 2 L flask fitted with a reflux condenser and magnetic stir-bar was introduced 2,5-dibromobenzoic acid (50.0 g, 0.1786 mol) and thionyl chloride (150 mL, 2.04 mol). The mixture was refluxed for 8 hours. Most of the thionyl chloride was distilled off followed by removal of the remainder by rotary evaporation. Distillation gave 40 g of 2,5-dibromobenzoyl chloride. (pot temperature 110° C.; distillation temp 70° C./0.70 mm Hg). Into a 2 L flask fitted with a reflux condenser and magnetic stir-bar The mixture was refluxed for 8 hours Most of the thionyl chloride was distilled off followed by removal of the remainder by rotary evaporation Distillation

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

実験手順: By the general method of Part C of Example 1, the reaction of 50.0 g (0.1786 mol) 2,5-dibromobenzoic acid with 150 mL thionyl chloride gave after distillation 40 g of 2,5-dibromobenzoyl chloride. gave after distillation 40 g of 2,5-dibromobenzoyl chloride

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

実験手順: 3,4-Dibromohexahydrophthalimide (0.10 mole), benzene (300 ml) and pyridine (0.11 mole) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. 2,5-Dibromobenzoyl chloride (0.10 mole) is then added dropwise to the flask with stirring at room temperature. After the addition is completed the reaction mixture is heated at reflux with continued stirring for a period of about 1 hour. After this time the reaction mixture is filtered and the filtrate is washed with water. The washed filtrate is then dried over anhydrous magnesium sulfate, filtered and stripped of solvent under reduced pressure to yield the desired product N-(2,5-dibromobenzoyl)-3,4-dibromohexahydrophthalimide. equipped with a mechanical stirrer thermometer and reflux condenser After the addition is heated at reflux with continued stirring for a period of about 1 hour After this time the reaction mixture is filtered the filtrate is washed with water The washed filtrate is then dried over anhydrous magnesium sulfate filtered

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

実験手順: Under a blanket of nitrogen, 2,5-dibromobenzoyl chloride (57.43 g, 0.11925 mol) was added to a solution of 4-octyloxybenzoic acid hydrazide (50.88 g, 0.1925 mol) and triethylamine (27 mL, 19.48 g, 0.1925 mol) in 800 mL of methylene chloride. The reaction mixture was stirred for 5 hours at room temperature. The precipitated solid was filtered off and re-crystallized from hot DMF/water gave 79.38 g (78% yield) 2,5-dibromo-N′-[4-(octyloxy)benzoyl]benzohydrazide. The precipitated solid was filtered off re-crystallized from hot DMF/water

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

実験手順: Into a 2 L flask fitted with a reflux condenser and magnetic stir-bar was introduced 2,5-dibromobenzoic acid (50.0 g, 0.1786 mol) and thionyl chloride (150 mL, 2.04 mol). The mixture was refluxed for 8 hours. Most of the thionyl chloride was distilled off followed by removal of the remainder by rotary evaporation. Distillation gave 40 g of 2,5-dibromobenzoyl chloride. (pot temperature 110° C.; distillation temp 70° C./0.70 mm Hg). Into a 2 L flask fitted with a reflux condenser and magnetic stir-bar The mixture was refluxed for 8 hours Most of the thionyl chloride was distilled off followed by removal of the remainder by rotary evaporation Distillation