반응 #2069246

ord-1e629998b0de4e64930cc97179c5810d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added
  2. 2
    기타reacted at a temperature of from 170° to 180° C. for 20 hours
  3. 3
    기타reacted at a temperature of from 120° to 130° C. for 3 hours
  4. 4
    기타the toluene layer was separated by liquid separation
  5. 5
    세척washed with water
  6. 6
    농축concentrated
  7. 7
    workup.DISTILLATIONpurified by distillation under reduced pressure

실험 절차

To a mixture of 58.5 g of N-acetyl-2,4-dimethoxyaniline and 70.7 g of bromobenzene, 29 g of anhydrous potassium carbonate, 2.1 g of copper powder and 0.8 g of iodine were added and reacted at a temperature of from 170° to 180° C. for 20 hours. Then, to this reaction mixture, 30 g of potassium hydroxide and 100 ml of isoamyl alcohol were added and reacted at a temperature of from 120° to 130° C. for 3 hours. To this reaction mixture, 300 ml of toluene was added, and the toluene layer was separated by liquid separation, washed with water, concentrated and then purified by distillation under reduced pressure, whereby 40 g of oily N-phenyl-2,4-dimethoxyaniline was obtained. The boiling point of this product was from 161° to 164° C./2 mmHg.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04594601uspto-grants-1986_06