반응 #1922811

ord-86f04b26e8e04787a808175bb016cfe7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타solution was transferred to a cylindrical funnel with pressure
  2. 2
    기타was kept in oil-bath at 85° C
  3. 3
    workup.ADDITIONwas poured out
  4. 4
    기타The reaction was terminated after that and the final
  5. 5
    기타reaction mixture
  6. 6
    기타to attain room temperature
  7. 7
    기타Product was separated by solvent evaporation
  8. 8
    기타The product was purified

실험 절차

4-Bromomethyl-2,6-di-tert-butyl-phenol (2.42 g, 0.008 mole) was dissolved in 50 mL of dry tetrahydrofuran. In a separate conical flask 2,5-dimethyl-benzene-1,4-diamine (2.17 g, 0.016 mole) was dissolved in 25 mL of tetrahydrofuran and solution was transferred to a cylindrical funnel with pressure equalizing tube. Three-necked round-bottom flask containing solution of 4-Bromomethyl-2,6-di-tert-butyl-phenol was kept in oil-bath at 85° C. Solution in the flask was continuously stirred with the help of magnetic stirrer. 2,5-dimethyl-para-phenylene diamine solution was added drop-by-drop, from funnel to the flask in acidic medium for a span of 4-5 hours till all the solution was poured out. The reaction was terminated after that and the final reaction mixture was allowed to attain room temperature. Product was separated by solvent evaporation. The product was purified using silica gel column chromatography. Product was identified by 1H-NMR. The yield of 4-[(4-Amino-2,5-dimethyl-phenylamino)-2,6di-tert-butyl-phenol is 1.86 g (65%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06770785B1uspto-grants-2004_08