تفاعل #302866

ord-9624ea7e963d448e9d21772267560ddb

معادلة التفاعل

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

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONmixed in an oil bath at 90° C
  2. 2
    أخرىafter about 30 minutes
  3. 3
    أخرىthe reaction was quenched
  4. 4
    درجة الحرارةThe cooled crude product
  5. 5
    غسيلwas base-washed twice through a solvent extraction
  6. 6
    غسيلwashed once with deionized water
  7. 7
    غسيلAfter washing
  8. 8
    تجفيفthe organic layer was dried with MgSO4
  9. 9
    ترشيحfiltered
  10. 10
    أخرىThe residual solution was dried
  11. 11
    أخرىa rotary evaporator
  12. 12
    أخرىto remove the solvent
  13. 13
    أخرىthe purified product was dried in a vacuum oven at 40° C. for 6 hours

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08192892B2uspto-grants-2012_06