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ChemicalBook CAS DataBase List Cantharidin

Cantharidin synthesis

9synthesis methods
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Yield:56-25-7 90%

Reaction Conditions:

Stage #1:furan;2,2,4,4-tetrahydrothiophene-3,4-dicarboxylic acid anhydride with 1-butyl-3-methylimidazolium Tetrafluoroborate at 50; for 19 h;
Stage #2: in ethyl acetate for 4 h;Reflux;Reagent/catalyst;Temperature;

Steps:

1.5 Preparation of cantharidin
To a 1 mL reaction vial, 26 mg of 2,5-dihydrothiophene-3,4-dicarboxylic anhydride, 91 μl of furan, 52 μl of 1-butyl-3-methylimidazolium tetrafluoroborate was added and the mixture was heated to 50 °C for 19 hours, Down to room temperature, 3 * 1 mL of ethyl acetate, Target HPLC 95% (2,5-dihydrothiophene-3,4-dicarboxylic anhydride content 0). The catalytic amount of Raney-Ni was refluxed for 4h, HPLC detection of cantharidin content 92%, filtration, 3*1mL ethyl acetate washing, Silica gel column separation of 30.8mg white crystals, cantharidin yield 90%

References:

Chongqing Traditional Chinese Medicine Institute;Liu Xiaoling;Tan Chunbin;Du Hongfei CN106674248, 2017, A Location in patent:Page/Page column 0027; 0036; 0037

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