反应 #302866

ord-9624ea7e963d448e9d21772267560ddb

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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