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ChemicalBook CAS DataBase List Mometasone furoate

Mometasone furoate synthesis

6synthesis methods
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Yield:83919-23-7 93.8%

Reaction Conditions:

with dichloro-hydantoin;acetic acid in butanone at -5 - 0; for 3 h;Reagent/catalyst;Solvent;

Steps:

1.5; 2.5

(5) Add 45g of compound V to 180mL of methyl ethyl ketone, stir and cool to -50 °C, add 5mL of glacial acetic acid, add 36g of dichlorohydantoin in four times at -50 °C, with an interval of 20 minutes each time, after adding, react at -50 °C for 3 hours, TLC tracked almost no raw materials, add dropwise 45mL of 30% sodium sulfite aqueous solution to quench the reaction, stir for 30 minutes, concentrate methyl ethyl ketone, filter, and dry the filter residue at 60 °C 10 hours, obtain 46 g of crude mometasone furoate, with a mass yield of 102.2% and a purity of 97.5%; add 45g crude mometasone furoate to 135mL dichloromethane and 90mL methanol, raise the temperature to 35-40°C, stir and dissolve, add 2.25g activated carbon to decolorize for 30 minutes, Filtration, concentration of the filtrate, centrifugal discharge, and drying at 60°C for 10 hours to obtain 42.2 g of mometasone furoate refined product, with a mass yield of 93.8%, a purity of 99.23%, and any impurity content less than 0.10%.

References:

CN113512085,2021,A Location in patent:Paragraph 0011-0012; 0037; 0041; 0046; 0048-0049; 0054

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