New downstream synthetic route of 145903-31-7

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Adding a certain compound to certain chemical reactions, such as: 145903-31-7, name is 7-Methoxy-2,3,4,5-tetrahydrobenzo[f][1,4]thiazepine, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 145903-31-7, HPLC of Formula: C10H13NOS

Synthon S26 was prepared according to methods described in U.S. patent application Ser. No. 10/680,988. Synthesis of S3 (Scheme 1): To a stirred solution of vinylsulfonic acid (22 mg, 0.2 mmol) in anhydrous CH2Cl2 (5 ml) is added thionyl chloride (2M in CH2Cl2, 0.1 ml, 0.2 mmol) The reaction mixture is stirred at room temperature overnight and evaporated under vacuum. The residue is dissolved in CH2Cl2 (5 ml). To this solution, a solution of S26 (20 mg, 0.1 mmol) in CH2Cl2 (3 ml) is added drop-wise at 0 C. The reaction mixture is stirred at 0 C. for one hour and at room temperature for another hour and washed with saturated sodium bicarbonate and 1N HCl. After removal of the solvent, the product S3 is purified by SiO2 column chromatography as a colorless oil (18 mg, 65%).

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Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; US2007/49572; (2007); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem