Synthesis method of Anagliptin key intermediate
A synthetic method and intermediate technology, applied in the field of drug synthesis, can solve the problems of less reported synthetic routes of pyrimidine-6-carboxylic acid, and achieve the effects of environmental friendliness, high product purity, and less side reactions
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Embodiment 1
[0042] 69.06g (1.0mol) of cyanoacetaldehyde, dissolved in 300ml of methanol, added 132g (1.1mol) of N,N-dimethylformamide dimethyl acetal, reacted at 20-25°C for 20-25h, and reduced Concentrate under reduced pressure to obtain an orange-yellow solid, which is recrystallized from ethanol to obtain a light yellow crystal, which is air-dried at 50°C for 10 hours to obtain 87 g of a solid, with a yield of 70%.
Embodiment 2
[0044] 69.06g (1.0mol) of cyanoacetaldehyde, dissolved in 400ml of ethanol, added 132g (1.1mol) of N,N-dimethylformamide dimethyl acetal, reacted at 20-25°C for 20-25h, and reduced Concentrate under reduced pressure to obtain an orange-yellow solid, which is recrystallized from ethanol to obtain light-yellow crystals, and air-dried at 50°C for 10 hours to obtain 75 g of solid, with a yield of 61.3%.
Embodiment 3
[0046] 69.06g (1.0mol) of cyanoacetaldehyde, dissolved in 550ml of isopropanol, add 132g (1.1mol) of N,N-dimethylformamide dimethyl acetal, react at 20-25℃ for 20-25h, end Concentrate under reduced pressure to obtain an orange-yellow solid, which is recrystallized from ethanol to obtain a light yellow crystal, which is air-dried at 50°C for 10 hours to obtain 76 g of a solid, with a yield of 70%.
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