반응 #60014

ord-eb6ad7a0b9d2406aad6f0d5931f4fdb6

반응 방정식

CCCCCCCCc1ccc(N)cc1
4-Octylaniline
C1COCCOCCOCCOCCOCCO1
18-crown-6
O=C([O-])[O-].[K+].[K+]
K2CO3
Clc1ccc(I)cc1
1-chloro-4-iodobenzene
CCCCCCCCc1ccc(N(c2ccc(Cl)cc2)c2ccc(Cl)cc2)cc1
bis(4-chlorophenyl)(4-octylphenyl)amine

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도to reflux for 24 hours under argon
  3. 3
    여과filtered
  4. 4
    기타After removal of solvent
  5. 5
    workup.DISTILLATIONby distillation
  6. 6
    기타the product was purified

실험 절차

4-Octylaniline (5.00 g, 244.4 mmol), 18-crown-6 (1.29 g, 4.9 mmol), K2CO3 (27.64 g, 194.8 mmol), 1-chloro-4-iodobenzene (14.51 g, 60.9 mmol, copper (6.19 g, 97.4 mmol), and 1,2-dichlorobenzene (100 mL) were added in a 250 mL flask with a condenser connected to a Dean Stark apparatus. The mixture was heated to reflux for 24 hours under argon. The reaction mixture was then cooled to room temperature, diluted with dichloromethane, and filtered. After removal of solvent by distillation, the product was purified using silica gel column chromatography using hexane as eluant. The yield was 4.18 g (40.3%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425723B2uspto-grants-2008_09