反应详情

温度

200 °C

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.

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