反応 #302866

ord-9624ea7e963d448e9d21772267560ddb

反応方程式

CC(C)(C)c1ccccc1O
t-butylphenol
Nc1ccccc1
aniline
CC(C)(C)c1ccccc1
t-BuPh

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONmixed in an oil bath at 90° C
  2. 2
    その他after about 30 minutes
  3. 3
    その他the reaction was quenched
  4. 4
    温度The cooled crude product
  5. 5
    洗浄was base-washed twice through a solvent extraction
  6. 6
    洗浄washed once with deionized water
  7. 7
    洗浄After washing
  8. 8
    乾燥the organic layer was dried with MgSO4
  9. 9
    ろ過filtered
  10. 10
    その他The residual solution was dried
  11. 11
    その他a rotary evaporator
  12. 12
    その他to remove the solvent
  13. 13
    その他the purified product was dried in a vacuum oven at 40° C. for 6 hours

実験手順

15 g (0.1 mol) of t-butylphenol, 6.31 g (0.21 mol) of p-formaldehyde and 10.24 g (0.11 mol) of aniline were added to a 100 ml one-neck round-bottom flask and mixed in an oil bath at 90° C. When the initially opaque mixture became a dark brown transparent gel type material after about 30 minutes, the reaction was quenched using tetrahydrofuran (THF), and then the mixture was cooled to room temperature. The cooled crude product was base-washed twice through a solvent extraction using a 1N NaOH aqueous solution, and washed once with deionized water. After washing, the organic layer was dried with MgSO4 and filtered. The residual solution was dried using a rotary evaporator to remove the solvent, and the purified product was dried in a vacuum oven at 40° C. for 6 hours to obtain t-BuPh-a.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08192892B2uspto-grants-2012_06