Preparation method of ceftiofur intermediate
A technology for ceftiofur and intermediates, which is applied in the field of preparation of ceftiofur intermediate cefuroxime, can solve the problems of difficult operation and high safety requirements for operators, and achieves reduced production cost, low cost and easy operability , the effect of optimizing the operating parameters
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[0025] Example 2 Preparation of furan-2-methylthiofuroic acid
[0024] Add water (2000mL) into the reaction flask, add sodium hydrosulfide (615.0g), stir until completely dissolved, cool to 5°C, add furoyl chloride (250.0g) dropwise, stir for 2h, add hydrochloric acid to adjust the pH to 1.0, Add ethyl acetate for extraction, separate the liquids and take the organic phase. Add anhydrous magnesium sulfate to dry. The yellow ethyl acetate solution was obtained by suction filtration, which was set aside.
Example Embodiment
[0025] Example 2 Preparation of furan-2-methylthiofuroic acid
[0026] Add water (1500mL) to the reaction flask, add sodium hydrosulfide (615.0g), stir until completely dissolved, cool to 0°C, add furoyl chloride (250.0g) dropwise, stir for 2h, add hydrochloric acid to adjust the pH to 1.5, Add methyl tert-butyl ether for extraction, add an equal volume of brine to the organic phase, stir for half an hour, then separate the liquids to take the organic phase. Add anhydrous magnesium sulfate to dry. Suction filtration to obtain a yellow methyl tert-butyl ether solution for use.
Example Embodiment
[0027] Example 3 Preparation of furan-2-methylthiofuroic acid
[0028] Add water (1000mL) into the reaction flask, add sodium hydrosulfide (307.5g), stir until completely dissolved, cool to 10°C, add furoyl chloride (250.0g) dropwise, stir for 3h, add hydrochloric acid to adjust the pH to 1.5, Add dichloroethane for extraction, add an equal volume of salt water to the organic phase, stir for half an hour, then separate the liquids to take the organic phase. Add anhydrous sodium sulfate to dry. Suction filtration to obtain a yellow dichloroethane solution for use.
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