80223-99-0Relevant articles and documents
Continuous-Flow Synthesis of (R)-Tamsulosin Utilizing Sequential Heterogeneous Catalysis
Ishitani, Haruro,Kobayashi, Shū,Laroche, Benjamin,Nishizawa, Ken,Saito, Yuki
, (2022/02/16)
We describe the continuous-flow synthesis of (R)-tamsulosin, a blockbuster therapeutic drug employed for dysuria associated with urinary stones and benign prostatic hyperplasia, by utilizing sequential heterogeneous catalysis. Two heterogeneous catalysts have been developed for the synthesis, and the key step involves reductive amination of nitriles using dimethylpolysilane-modified Pd on activated carbon/calcium phosphate. Overall, (R)-tamsulosin was obtained in 60 % yield and 64 % ee (99 % ee after recrystallization) in a flow stream through four catalytic transformations without the need for the isolation or purification of any intermediates or byproduct.
Preparation method of tamsulosin hydrochloride crystal form
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Paragraph 0017-0020, (2021/05/26)
The invention relates to the technical field of preparation of crystal forms of organic compounds, in particular to a preparation method of a tamsulosin hydrochloride crystal form. The method comprises the following steps: completely dissolving tamsulosin in a solvent at 60-70 DEG C, then dropwise adding acid for reaction for a period of time, conducting cooling to 20-30 DEG C, and conducting filtering, washing and drying to obtain tamsulosin, wherein tamsulosin is a refined product. The method is simple in process, high in yield, high in product purity and suitable for large-scale industrialization.
A high optical purity of tamsulosin preparation method of leach
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Paragraph 0037; 0040; 0043; 0044; 0045; 0046; 0049, (2018/10/02)
The invention discloses a preparation method of tamsulosin hydrochloride with high optical purity, and belongs to a medicine technology and a chemical field. A recrystallization method is adopted, crude products of (R)-5-(2-(2-(2-ethoxyphenoxy) ethyl amino) propyl)-2-methoxyl phenyl sulfonamide hydrochloride are refined, so that pure products of the (R)-5-(2-(2-(2-ethoxyphenoxy) ethyl amino) propyl)-2-methoxyl group sulfonamide hydrochloride of which the e.e. value is larger than 99.8% is obtained; a crystallizing solvent adopted by the recrystallization method is a mixed solvent consisting of an organic solvent and water, the organic solvent is selected from one of methanol, ethyl alcohol, acetone, acetonitrile and isopropyl alcohol, and the recrystallization temperature is under 15 DEG C. The preparation method disclosed by the invention is simple to operate, short in period, low in cost and good in repeatability, and can solve the inevitable problem of rework for treatment in the industrial production.