A kind of method reducing methylene chloride residual amount in ampicillin
A technology of ampicillin and dichloromethane, which is applied in the field of reducing the residual amount of dichloromethane in ampicillin, can solve the problems of affecting economic benefits, the decline of amoxicillin yield, and the inability to balance quality and yield, and achieve a large yield , the effect of high purity
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Embodiment 1
[0038]Add 100mL of the primary aqueous phase obtained in the hydrolysis process in the chemical synthesis of ampicillin into the reactor; according to the volume ratio of the solvent and the primary aqueous phase being 1.0, add 100mL of n-hexane to extract the primary aqueous phase of ampicillin. At this time, the primary aqueous phase of ampicillin is The residual dichloromethane in the phase is 15000ppm; the mixed solution is stirred rapidly at 13°C for 20min, and after standing for 10min, the phases are separated to obtain a secondary aqueous phase and a secondary organic phase. The secondary aqueous phase is mainly ampicillin. At this time The residual dichloromethane in the secondary water phase is 550ppm; therefore, when the volume ratio of n-hexane to the primary water phase is 1.0, the removal rate of dichloromethane is 95.51% when n-hexane is applied mechanically once. The secondary organic phase is mainly n-hexane; the secondary aqueous phase containing ampicillin is ...
Embodiment 2
[0041] Add 100mL of the primary water phase obtained in the hydrolysis process in the chemical synthesis of ampicillin into the reactor; according to the volume ratio of the solvent and the primary water phase of 0.4, add 40mL of n-heptane to extract the primary water phase of ampicillin, and at this time, the primary water phase of ampicillin is The dichloromethane residue in the water phase was 16000ppm; the mixed solution was stirred rapidly at 15°C for 10 minutes, and after standing for 10 minutes, the phases were separated to obtain a secondary water phase and a secondary organic phase. The secondary water phase was mainly ampicillin. When the dichloromethane residue in the secondary water phase is 350ppm; therefore when the volume ratio of n-heptane to the primary water phase is 0.4, the removal rate of dichloromethane when n-heptane is applied mechanically once is 97.8%. The secondary organic phase is mainly n-heptane; the secondary aqueous phase containing ampicillin is...
Embodiment 3
[0044] Add 100mL of the primary aqueous phase obtained in the hydrolysis process in the chemical synthesis of ampicillin into the reactor; according to the volume ratio of the solvent and the primary aqueous phase of 0.6, add 60mL of ethyl acetate to extract the primary aqueous phase of ampicillin, and at this time, the primary aqueous phase of ampicillin is The residual dichloromethane in the water phase was 15000ppm; the mixed solution was stirred rapidly at 10°C for 20 minutes, and after standing for 15 minutes, the phases were separated to obtain a secondary water phase and a secondary organic phase. The secondary water phase was mainly ampicillin. The residual dichloromethane in the secondary water phase is 400ppm, so when the volume ratio of ethyl acetate to the primary water phase is 0.5, the removal rate of dichloromethane is 97.3% when ethyl acetate is applied mechanically once. The secondary organic phase is mainly ethyl acetate; the secondary aqueous phase containing...
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