New preparation technique of urapidil hydrochloride
A technology of urapidil hydrochloride and preparation process, applied in the field of pharmaceutical synthesis, can solve problems such as water environment pollution, and achieve the effects of easy post-processing, less side reactions and high yield
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Embodiment 1
[0036] Embodiment 1 The new preparation technology of urapidil hydrochloride of the present invention
[0037] A. Under nitrogen protection, in a 50L reactor, add 1,3-bis(2,6-diisopropylphenyl)imidazolium chloride (8.50g, 0.02mol), Pd(OAc) in sequence 2 (2.25g, 0.01mol), degassing solvent dioxane (20L) and potassium carbonate (691.1g, 5.0mol) stirred at room temperature and reacted for 0.5h (stirring speed 120r / min), after adding 1-(2-formazan Oxyphenyl)piperazine hydrochloride (571.8g, 2.5mol), 6-(3-chloropropyl)-1,3-dimethyluracil (634.4g, 2.75mol), heated for 6h (stirring speed 120r / min, heating temperature 80°C), after cooling to room temperature, a solid precipitated, filtered under reduced pressure (vacuum degree -0.08MPa~0.1MPa) to obtain the crude product, the crude product was dissolved in 20L of hot ethanol (temperature 70°C) Afterwards, filter while it is hot, and the filtrate stands overnight for 12 hours to obtain white crystals. The filter cake is filtered under...
Embodiment 2
[0043] Embodiment 2 The new preparation technology of urapidil hydrochloride of the present invention
[0044] The difference between this embodiment and embodiment 1 is that the A step uses PdCl 2 (1.77g, 0.01mol) instead of Pd(OAc) 2 (2.25g, 0.01mol), degassing solvent tetrahydrofuran (20L) instead of degassing solvent dioxane (20L), to obtain urapidil 783.6g, yield 81.1%, melting range 157-158 ℃; B step with methanol / isopropanol mixed solvent (20L, V 甲醇 :V 异丙醇 =1:1) instead of methanol / ethanol mixed solvent (20L, V 甲醇 :V 乙醇 =1:1); The present embodiment obtains 304.5 g of urapidil hydrochloride, and the crystallization yield is 72.0%. The total yield is 58.4%, the content of related substances is 0.0041%, and the spectral data are the same as in Example 1.
Embodiment 3
[0045] Embodiment 3 The new preparation technology of urapidil hydrochloride of the present invention
[0046] The difference between this embodiment and embodiment 1 is that the A step uses PdCl 2 (1.77g, 0.01mol) instead of Pd(OAc) 2 (2.25g, 0.01mol), with sodium carbonate (530.0g, .5.0mol) instead of potassium carbonate (691.1g, 5.0mol), degassed tetrahydrofuran (20L) instead of degassed dioxane (20L), to uradi Mole 795.2g, yield 82.3%, melting range 157-158 ℃; B step uses methanol / acetone mixed solvent (20L, V 甲醇 :V 丙酮 =1:1) instead of methanol / ethanol mixed solvent (20L, V 甲醇 :V 乙醇 =1:1); The present embodiment obtains 313.4 g of urapidil hydrochloride, and the crystallization yield is 74.1%. The total yield is 61.0%, the content of related substances is 0.0040%, and the spectral data are the same as in Example 1.
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