Dess-Martin Periodinane CAS 87413-09-0 (DMP) Assay >98.0% (Base on Theoxidation) Factory

2-Iodobenzoic Acid (50.0g, 0.20mol) was added to sulfolane (250mL), the solution was heated to 50℃. 90% of the above solution was slowly added dropwise to an aqueous solution (147.4 ml) of potassium hydrogen persulfate (0.24g, 1.2 mol, eq) at 50℃, and the reaction was incubated for 3 hours. Subsequently, the reaction solution was heated to 95℃. And the remaining 10% 2-iodobenzoic acid solution was slowly added dropwise to the reaction solution, and the reaction was continued for 3 hours. After completion of the reaction, it was cooled to 5℃ and stirring was continued at this temperature for 1.5 hours. 1L of water was added with stirring and filtered (the filtrate was to be recycled). The filter cake was rinsed with water and acetone successively and dried at room temperature for 16 hours to obtain 53.2g of 2-iodoylbenzoic acid (yield: 95.04%), white solid with 99.7% purity (confirmed by NMR and HPLC). Detected by HNMR, The solid was determined to be 2-iodoylbenzoic acid. 2-iodoylbenzoic acid (45g, 0.16mol) was added to acetic anhydride (49G, 0.48mol) and dioxane (90ml), followed by B(C6F5)3 (0.0016mol), the reaction solution was heated to 50℃. And stirred for 10 minutes, and then the solvent was distilled off under reduced pressure. The reaction solution was added with methyl tert-butyl ether (400mL), suction filtered, and dried at room temperature to obtain a white solid (61.1g, yield: 90%). The purity was 99.1% (confirmed by NMR).