反应 #1306911
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04288592
反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Acetyl chloride (2.13 mls; 0.03 mole) is added dropwise to a suspension of 2,4,5-trichloroaniline (4.91 g; 0.025 mole) and powdered 3A molecular sieves (7.4 g) in dichloromethane (25 mls), at room temperature, under a nitrogen atmosphere. When addition is completed, the mixture is heated to 50° C. for 1.5 hours and then cooled to room temperature. The 3A sieves are separated by filtration and washed with dichloromethane. All dichloromethane solutions are combined and evaporated to obtain 4.1 grams (69% of theoretical) of the solid product; m.p. 188°-190° C. after recrystallized from toluene. at room temperature When addition cooled to room temperature The 3A sieves are separated by filtration washed with dichloromethane evaporated to obtain 4.1 grams (69% of theoretical) of the solid product m.p. 188°-190° C. after recrystallized from toluene
来源 ID: ord-55fa5f57c1224c8aa63b76b6d398bdcc