反応 #1079378

反応方程式

1,5-bis(phenylamino)naphthalene

p-iodotoluene

potassium carbonate

nitrobenzene

1,5-diamino naphthalene

iodobenzene

potassium carbonate

nitrobenzene

→

1,5-bis(Phenyl-p-tolylamino)naphthalene

溶媒

toluene

toluene

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   ろ過followed by filtration for removal of inorganic compounds
3. 3
   その他Toluene and nitrobenzene were removed by distillation in a reduced pressure ambient
4. 4
   その他the remainder was subjected to separation refinement in a silica gel column
5. 5
   その他to 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
   ろ過followed by filtration for removal of inorganic compounds
9. 9
   その他Toluene and nitrobenzene were removed by distillation in a reduced pressure ambient
10. 10
    その他the remainder was subjected to separation refinement in a silica gel column
11. 11
    その他to prepare 7 gram of 1,5-bis(phenyl-p-tolylamino)naphthalene

実験手順

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.

出典