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The production process of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine (CAS 101251-50-5) involves several steps, including the synthesis of the starting materials, the reaction of the starting materials to form the product, and the purification of the product.
- Synthesis of starting materials
The synthesis of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine begins with the synthesis of the starting materials, which include 4-chloro-6-(2,4-dihydroxy-6-methyl-3-pyridine)-1,3-oxazepan-2-amine and 2,4-dichloro-6-methyl-1,3,5-triazine.
The synthesis of 4-chloro-6-(2,4-dihydroxy-6-methyl-3-pyridine)-1,3-oxazepan-2-amine involves the reaction of 2,6-dimethylphenylamine with sodium hydroxide and 2,4-dichlorophenyl isocyanate in the presence of an alkali metal carbonate, such as sodium carbonate.
This reaction is followed by the reduction of the resulting oxazepane with lithium aluminum hydride.
The synthesis of 2,4-dichloro-6-methyl-1,3,5-triazine involves the reaction of 2,4-dimethylphenylamine with chloroacetyl chloride in the presence of a base, such as sodium hydrogen carbonate.
This reaction is followed by the reduction of the resulting nitrile with lithium aluminum hydride.
- Synthesis of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine
The synthesis of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine involves the reaction of 4-chloro-6-(2,4-dihydroxy-6-methyl-3-pyridine)-1,3-oxazepan-2-amine and 2,4-dichloro-6-methyl-1,3,5-triazine in the presence of a base, such as sodium hydrogen carbonate.
The reaction is typically carried out in an organic solvent, such as dichloromethane or chloroform, at a temperature of around 0°C to 10°C.
The reaction is typically complete within 1 to 2 hours.
- Purification of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine
After the synthesis of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine, the product is typically purified by precipitation with a polar solvent, such as ethyl acetate or ethanol.
The precipitated solid is then dried and suspended in a non-polar solvent, such as ether or hexane, and filtered to remove any impurities.
The filtrate is then evaporated to dryness to obtain a pure sample of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine.
The total yield of 4,4'-(6-chloropyrimidine-2,4-diyl)dihydro-2H-pyrimidine can
