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The production process of (6-chloro-2-methanesulfonyl-pyrimidin-4-yl)-ethyl-amine, also known as MCI-290, involves several steps that require careful control and optimization.
This article will provide a detailed overview of the production process of this important Raw Material in the chemical industry.
Step 1: Preparation of 2-methanesulfonyl-pyrimidine
The first step in the production of MCI-290 involves the preparation of 2-methanesulfonyl-pyrimidine.
This compound is typically synthesized by reacting 2-methylthio-pyrimidine with methylsulfonyl chloride in the presence of a solvent such as DMF.
The reaction is typically carried out at a temperature of around 60°C for several hours, after which the solvent is removed under reduced pressure, and the residue is purified by chromatography.
Step 2: Nitration of 2-methanesulfonyl-pyrimidine
Once 2-methanesulfonyl-pyrimidine has been prepared, it is subjected to nitration to produce 2-methanesulfonyl-pyrimidine-NONOate.
This is typically done by adding nitrating acid, such as fuming nitric acid, to a solution of the compound in a solvent such as acetonitrile.
The reaction is typically carried out at a temperature of around 0°C, and the solvent is removed under reduced pressure after the reaction is complete.
Step 3: N-Ethylation of 2-methanesulfonyl-pyrimidine-NONOate
The next step is the N-ethylation of 2-methanesulfonyl-pyrimidine-NONOate, which involves the addition of ethyl iodide to the compound.
This reaction is typically carried out in the presence of a solvent such as THF and a base such as sodium hydride.
The reaction is typically carried out at a temperature of around 60°C for several hours, after which the solvent is removed under reduced pressure, and the residue is purified by chromatography.
Step 4: Deprotection of N-Ethylated Product
In this step, the N-ethyl group is removed from the N-ethylated product, which is achieved by treating the material with a base such as sodium hydroxide in a solvent such as methanol.
The reaction is typically carried out at a temperature of around 50°C for several hours, after which the solvent is removed under reduced pressure, and the residue is purified by chromatography.
Step 5: Ketylation of N-Deprotected Product
The N-deprotected product is then subjected to ketylation to produce the final product, MCI-290.
This is typically done by adding a ketone such as acetone to a solution of the compound in a solvent such as THF.
The reaction is typically carried out at a temperature of around 50°C for several hours, after which the solvent is removed under reduced pressure, and the residue is purified by chromatography.
Quality Control
Throughout the production process, it is essential to monitor the quality of the raw materials and intermediates used, as well as the final product.
This can be achieved by using a variety of analytical techniques, such as mass spectrometry, nuclear magnetic resonance spectroscopy, and chromatography.
In addition, regular testing and monitoring of the product can help ensure that it meets the required specifications for purity and potency.
Conclusion
The production process of MCI-290 involves several steps that require careful control and optimization.
From the preparation of 2-methanesulfonyl-pyrimidine to the final step of ket