Preparation process of ticarcillin disodium salt
A technology of ticarcillin disodium salt and ticarcillin acid, applied in the field of preparation of penicillin antibiotics ticarcillin disodium salt, can solve the problems of high water content, freeze-drying method does not separate impurities, and harsh operation requirements
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Embodiment 1
[0033] At 0°C, extract the reaction solution containing 50g of ticarcillinic acid twice with 50mL×2 butyl acetate, combine the butyl acetate extracts, dilute with 50mL of acetone, add 2g of activated carbon, decolorize for 30min, filter, and Add an acetone solution of sodium isooctanoate to the mother liquor, add seed crystals, stir and grow the crystals at 10°C for 2.5 hours, then slowly add 100mL of acetone, after the addition is complete, filter under reduced pressure, and dry in vacuum at 80°C to obtain white ticarcillin disodium Salt, yield 78%; 1 HNMR (D20): 7.44 (m, 1H), 7.34 (m, 1H), 7.13 (m, 1H), 5.58 (d, 1H), 5.47 (d, 1H), 4.68 (m, 1H), 4.24 (m , 1H), 1.5(m, 6H).
Embodiment 2
[0035] At 50°C, extract the reaction solution containing 10 g of ticarcillinic acid twice with 10 mL×2 butyl acetate, combine the butyl acetate extracts, dilute with 50 mL of butyl acetate, add 0.5 g of activated carbon, and decolorize for 30 min. Filtrate, add sodium isocaproate acetone solution to the mother liquor, add seed crystals, stir and grow crystals at 5°C for 2.5h, then slowly add 500mL of acetone, after addition, filter under reduced pressure, vacuum dry at 40°C to obtain white ticar Cillin disodium salt, HPLC purity 99.1%, maximum impurity 0.4%.
Embodiment 3
[0037] At -5°C, extract the reaction solution containing 5g ticarcillinic acid twice with 10mL×2 dichloromethane, combine the dichloromethane extracts, dilute with 10mL methanol, add 0.2g activated carbon, decolorize for 30min, and filter , add methanol solution of sodium methoxide to the mother liquor, add seed crystals, stir and grow crystals at 10°C for 2.5h, then slowly add 500mL of acetone, after addition, filter under reduced pressure, vacuum dry at 20°C to obtain white ticarcillin di Sodium salt, HPLC purity 99.0%, maximum impurity 0.3%.
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