تفاعل #1079378

ord-ffdd0ddee9ae40e1a80bf09ab9ee792c

المذيبات

ظروف التفاعل

درجة الحرارة
200°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    ترشيحfollowed by filtration for removal of inorganic compounds
  3. 3
    أخرىToluene and nitrobenzene were removed by distillation in a reduced pressure ambient
  4. 4
    أخرىthe remainder was subjected to separation refinement in a silica gel column
  5. 5
    أخرىto prepare 10 gram of 1,5-bis(phenylamino)naphthalene
  6. 6
    workup.STIRRINGfor stirring at 200° C. for 30 hours
  7. 7
    workup.ADDITIONwas added
  8. 8
    ترشيحfollowed by filtration for removal of inorganic compounds
  9. 9
    أخرىToluene and nitrobenzene were removed by distillation in a reduced pressure ambient
  10. 10
    أخرىthe remainder was subjected to separation refinement in a silica gel column
  11. 11
    أخرىto prepare 7 gram of 1,5-bis(phenyl-p-tolylamino)naphthalene

الإجراء التجريبي

8 gram (0.05 mol) of 1,5-diamino naphthalene, 22 gram (0.11 mol) of iodobenzene, 17 gram (0.12 mol) of potassium carbonate, 0.4 gram of copper powder and 50 milliliter of nitrobenzene were introduced in a 100 milliliter three-necked flask for stirring at 200° C. for 30 hours. After the reaction, toluene was added, followed by filtration for removal of inorganic compounds. Toluene and nitrobenzene were removed by distillation in a reduced pressure ambient, and the remainder was subjected to separation refinement in a silica gel column using a 1:3 mixture solvent of toluene and ligroin, to prepare 10 gram of 1,5-bis(phenylamino)naphthalene. Thereafter, 6.2 gram (0.02 mol) of 1,5-bis(phenylamino)naphthalene, 11 gram (0.05 mol) of p-iodotoluene, 7 gram (0.05 mol) of potassium carbonate, 0.3 gram of copper powder and 50 milliliter of nitrobenzene were introduced in a 100 milliliter three-necked flask for stirring at 200° C. for 30 hours. After the reaction, toluene was added, followed by filtration for removal of inorganic compounds. Toluene and nitrobenzene were removed by distillation in a reduced pressure ambient, and the remainder was subjected to separation refinement in a silica gel column using a 1:3 mixture solvent of toluene and ligroin, to prepare 7 gram of 1,5-bis(phenyl-p-tolylamino)naphthalene.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06468675B1uspto-grants-2002_10