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Instructions for the synthesis of 2,7-Dibromo-N-phenylcarbazole:
- Prepare a solution of N-phenylcarbazide in a suitable solvent, such as DMF or acetonitrile.
The concentration of the solution should be approximately 1-5 M. - Add a solution of NaBr in water to the solution of N-phenylcarbazide, stirring constantly.
The concentration of the NaBr solution should be approximately 5-10 M. - Continue stirring the mixture for several hours, until the reaction is complete.
This can be determined by TLC or HPLC analysis. - Pour the reaction mixture into a separatory funnel and add a small amount of water.
Shake the mixture vigorously, then allow it to settle.
Draw off the lower layer and rinse the residue with a small amount of water. - Transfer the organic layer to a dry, round-bottomed flask equipped with a magnetic stirrer and a condenser.
- Add a solution of K2CO3 in water to the organic layer, stirring constantly.
The concentration of the K2CO3 solution should be approximately 5-10 M. - Continue stirring the mixture for several hours, until the reaction is complete.
This can be determined by TLC or HPLC analysis. - Pour the reaction mixture into a separatory funnel and add a small amount of water.
Shake the mixture vigorously, then allow it to settle.
Draw off the lower layer and rinse the residue with a small amount of water. - Transfer the organic layer to a dry, round-bottomed flask equipped with a magnetic stirrer and a condenser.
- Add a solution of NaI in water to the organic layer, stirring constantly.
The concentration of the NaI solution should be approximately 5-10 M. - Continue stirring the mixture for several hours, until the reaction is complete.
This can be determined by TLC or HPLC analysis. - Pour the reaction mixture into a separatory funnel and add a small amount of water.
Shake the mixture vigorously, then allow it to settle.
Draw off the lower layer and rinse the residue with a small amount of water. - Transfer the organic layer to a dry, round-bottomed flask equipped with a magnetic stirrer and a condenser.
- Add a solution of Na2CO3 in water to the organic layer, stirring constantly.
The concentration of the Na2CO3 solution should be approximately 5-10 M. - Continue stirring the mixture for several hours, until the reaction is complete.
This can be determined by TLC or HPLC analysis. - Pour the reaction mixture into a separatory funnel and add a small amount of water.
Shake the mixture vigorously, then allow it to settle.
Draw off the lower layer and rinse the residue with a small amount of water. - Transfer the organic layer to a dry, round-bottomed flask equipped with a magnetic stirrer and a condenser.
- Add a solution of MgSO4 in water to the organic layer, stirring constantly.
The concentration of the MgSO4 solution should be approximately 5-10 M. - Continue stirring the mixture for several hours, until the reaction is complete.
This can be determined by TLC or HPLC analysis. - Pour the reaction mixture into a separatory funnel and add a small amount of water.
Shake the mixture vigorously, then allow it to settle.
Draw off the lower layer and rinse the residue with a small amount of water. - Transfer the organic layer to a dry, round-bottomed flask equipped with a magnetic stirrer and a condenser.
- Add a solution of NaCl in water to the organic layer, stirring constantly.
The concentration of the NaCl