Dissociation method and application of titanium complex drug
A drug and complexing technology, applied in the direction of organic chemistry, etc., can solve the problems of inability to provide products with good quality, increase the difficulty of product purification, and low yield of target substances.
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Embodiment 1
[0040] (1) Add 50 g of titanium tetrachloride to the solution of 60 g of A, and react for 1 hour;
[0041] (2) Pour the reaction solution into 300ml of 1% isopropanol solution and stir for 0.5 hours;
[0042] (3) Add 200g 40% citric acid solution, pH<4, stir for 0.5 hours;
[0043] (4) Layering and concentration of the organic layer to obtain (3S, 4S)-4-acetyl-3-((R)-1-hydroxyethyl)-1-(4-methoxyphenyl) nitrogen heterocycle Butan-2-one 40g, yield 66.7%, purity 99.5%.
Embodiment 2
[0045] (1) Add 50 g of titanium tetrachloride to the solution of 60 g of A, and react for 1 hour;
[0046] (2) Pour the reaction solution into 300ml of 1% isopropanol solution and stir for 0.5 hours;
[0047] (3) Add 250g 40% citric acid solution, pH<4, stir for 0.5 hours;
[0048] (4) Layering and concentration of the organic layer to obtain (3S, 4S)-4-acetyl-3-((R)-1-hydroxyethyl)-1-(4-methoxyphenyl) nitrogen heterocycle Butan-2-one 42g, yield 70%, purity 99.7%.
Embodiment 3
[0050] (1) Add 50 g of titanium tetrachloride to the solution of 60 g of A, and react for 1 hour;
[0051] (2) Pour the reaction solution into 300ml 0.5% isopropanol solution and stir for 0.5 hour;
[0052] (3) Add 250g 40% citric acid solution, pH<4, stir for 0.5 hours;
[0053] (4) Layering and concentration of the organic layer to obtain (3S, 4S)-4-acetyl-3-((R)-1-hydroxyethyl)-1-(4-methoxyphenyl) nitrogen heterocycle Butan-2-one 45g, yield 75%, purity 99.7%.
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