The Production Process of Urea, N′-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-N-(2-chloroethyl)-N-nitroso-, hydrochloride (1:1)

Urea, N′-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-N-(2-chloroethyl)-N-nitroso-, hydrochloride (1:1) is a synthetic chemical compound that is commonly used in various industrial processes.
The production process of this compound involves several steps, which are carefully designed to optimize the yield and purity of the final product.
In this article, we will discuss the production process of urea, N′-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-N-(2-chloroethyl)-N-nitroso-, hydrochloride (1:1) in detail.

Step 1: Preparation of N-(2-chloroethyl)nitrosourea
The production of urea, N′-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-N-(2-chloroethyl)-N-nitroso-, hydrochloride (1:1) begins with the preparation of N-(2-chloroethyl)nitrosourea.
This compound is synthesized by reacting sodium nitrite with 2-chloroethyl chloride in the presence of a solvent such as acetonitrile or dichloromethane.
The reaction is typically carried out at room temperature and is followed by the addition of water to the reaction mixture to obtain a clear solution.

Step 2: Addition of N-methylpyrrolidine
After the preparation of N-(2-chloroethyl)nitrosourea, the next step involves the addition of N-methylpyrrolidine to the solution.
This compound is added to the solution to catalyze the reaction between N-(2-chloroethyl)nitrosourea and ammonia.
The reaction is carried out at a temperature between 50°C and 70°C, and the mixture is stirred for several hours to ensure complete reaction.

Step 3: Neutralization with Ammonia
After the addition of N-methylpyrrolidine, the solution is neutralized with ammonia.
This step is carried out by adding ammonia to the solution slowly while stirring the mixture.
The reaction is allowed to proceed for several hours, and the mixture is then filtered to remove any solids that may have formed.

Step 4: Purification of the Product
The product obtained from the previous step is purified by recrystallization.
This involves dissolving the crude product in a solvent such as ethanol or acetonitrile and allowing it to crystallize slowly.
The crystals are then filtered, washed with a solvent such as hexane, and dried to obtain pure N-(2-chloroethyl)nitroso-N-(4-amino-2-methyl-5-pyrimidinyl)urea.

Step 5: Hydrolysis of N-(2-chloroethyl)nitroso-N-(4-amino-2-methyl-5-pyrimidinyl)urea
The final step in the production of urea, N′-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-N-(2-chloroethyl)-N-nitroso-, hydrochloride (1:1) involves the hydrolysis of N-(2-chloroethyl)nitroso-N-(4-amino-2-methyl-5-pyrimidinyl)urea in the presence of water.
This step is carried out by adding water to the crude product and allowing it to react with the water.
The reaction is allowed to proceed for several hours, and the mixture is then filtered to remove any solids that may have formed.

The crude product obtained from the hydrolysis step is then further purified by recrystallization or column chromatography.
This involves dissolving the crude product in a solvent such as ethanol or acetonitrile and allowing it to crystallize slowly.
The crystals are then filtered, washed with a solvent such as hexane, and dried to obtain pure urea, N′-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-N-(2-chloro