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In the Chemical Industry, efficient and cost-effective processes are always in high demand.
One such process that has gained recent attention is the synthesis of 5-Bromo-3-(trifluoromethyl)-2-pyridinecarbonitrile, commonly referred to as 5-BTBPC.
This article will delve into the synthesis of 5-BTBPC and the instructions for the successful synthesis of this compound.
Synthesis of 5-BTBPC:
The synthesis of 5-BTBPC can be achieved through multiple methods, but the most efficient method is the synthesis of 2-Chloropyridine-3-boronic acid salt, followed by its reduction with Lithium Aluminum Hydride (LiAlH4) and subsequent bromination with N-Bromosuccinimide (NBS).
This synthesis process involves several steps and requires the use of specialized equipment and chemicals.
Step 1: Preparation of 2-Chloropyridine-3-boronic acid salt
In this step, 2-Chloropyridine is treated with Boric acid and sodium hydroxide, and the resulting salt is then treated with a base, such as sodium carbonate to neutralize the acid.
The resulting salt can then be extracted with an organic solvent, such as ethyl acetate, to remove the boric acid.
This salt is then used as the starting material for the next step.
Step 2: Reduction with Lithium Aluminum Hydride (LiAlH4)
In this step, the 2-Chloropyridine-3-boronic acid salt is treated with LiAlH4, which reduces the boronic acid to form the 2-Chloropyridine-3-amino acid.
The reduction is typically carried out in the presence of a solvent, such as ethanol or tetrahydrofuran, and a catalyst, such as Catalyst A or Catalyst B.
The reduction step can be time-consuming and requires careful monitoring to ensure that the reaction is proceeding as expected.
Step 3: Bromination with N-Bromosuccinimide (NBS)
In this step, NBS is added to the 2-Chloropyridine-3-amino acid and the reaction is typically carried out in the presence of a solvent, such as benzene or toluene.
The reaction generates a large amount of heat and requires careful monitoring to prevent overheating.
The reaction can also be accompanied by the formation of secondary products, which can adversely affect the yield of the desired product.
Overall, the synthesis of 5-BTBPC requires careful planning and execution and can be time-consuming and costly.
The successful synthesis of this compound relies on the proper preparation of the starting material, the careful monitoring of the reaction conditions, and the use of specialized equipment and chemicals.
Instructions for the Synthesis of 5-BTBPC:
The following are general instructions for the synthesis of 5-BTBPC:
- Prepare 2-Chloropyridine-3-boronic acid salt in an air-free, dry, and well-ventilated area, using appropriate safety equipment.
- Reduce the 2-Chloropyridine-3-boronic acid salt using LiAlH4 in the presence of a solvent and a catalyst.
- Brominate the 2-Chloropyridine-3-amino acid using NBS in the presence of a solvent.
- Purify the resulting product using standard purification methods, such as recrystallization or chromatography.
- Characterize the product using standard characterization methods, such as mass spectrometry or nuclear magnetic resonance spectroscopy.
It is important to note that the synthesis of 5-BTBPC and the preparation of the starting material, as well as the handling