Preparation method of pentafluorophenyl methanesulfonate
A technology of pentafluorophenyl methanesulfonate and methanesulfonic anhydride is applied in the field of preparation of pentafluorophenyl methanesulfonate, and can solve the problems of easily causing danger, potential safety hazard, easy introduction of chloride ions, and the like, To achieve the effect of easy transportation and storage, reduced difficulty and cost, and simple purification process
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[0037] (1) Synthesis of Pentafluorophenyl Methanesulfonate
[0038] Take by weighing 50g pentafluorophenol (0.272mol) and certain quality methanesulfonic anhydride (by the proportioning in the specific example in the table) respectively in the glove box, and be dissolved in the organic solvent of 200ml respectively; Pentafluorophenol / Organic solvent was added to a three-necked flask, and 80ml of acid-binding agent was added at the same time; under normal temperature and nitrogen protection, methanesulfonic anhydride / organic solvent was added dropwise, and the dropping time was 5h. After the dropwise addition, adjust the temperature to 50°C and continue the reaction for 24h.
[0039] (2) purification of pentafluorophenyl methanesulfonate
[0040] There are two main purification methods of pentafluorophenyl methanesulfonate:
[0041] Method 1: After the crude pentafluorophenyl methanesulfonate is prepared, the temperature of the reaction solution is lowered to -5-5°C, the rea...
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