Reaction #2203036
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04493883
Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: There was prepared (3-phthalimidopropyl)trimethylammonium tetrafluoroborate by dissolving 145 grams, 1.42 moles, of dimethylaminopropylene, and 3.92 grams, 0.039 moles of triethylamine in one liter of xylene, in a two litered three necked round bottom flask equipped with a stirrer, a thermometer, a heating mantle, a Dean-Stark trap, and a reflux condenser. Subsequently 191.3 grams, 1.29 moles of phthalic anhydride was added, and the mixture was refluxed at a temperature of 140 degrees centigrade. Subsequent to refluxing for 24 hours, 24 milliliters of water was collected in the Dean-Stark trap. The xylene and excess amines were then removed from the reaction mixture on a rotary evaporator yielding the crude product N-(dimethylaminopropyl)phthalimide, in a yield of 300 grams. The crude imide separated was a brown syrup which crystallized on standing. This imide product, subsequent to purification by vacuum distillation, was identified by elemental analysis and infrared spectroscopy. by dissolving 145 grams, 1.42 moles the mixture was refluxed at a temperature of 140 degrees centigrade Subsequent to refluxing for 24 hours 24 milliliters of water was collected in the Dean-Stark trap The xylene and excess amines were then removed from the reaction mixture on a rotary evaporator
Source ID: ord-da799152df1d4a13bc257db9aec15479