Method for preparing penam sulfoxide acid diphenyl methyl ester which is tazobactam precursor
A technology of diphenylmethyl sulfoxide and aminopenicillanic acid is applied in the field of synthesis of tazobactam pharmaceutical intermediates, and can solve the problems of potential safety hazards, high cost, poor safety and reliability, etc. The effect of reducing the discharge of three wastes and improving process safety
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[0038] Example 1
[0039] 1). Add 500L of dichloromethane, 180kg of water to a 1500L reactor, add 120kg of 6-aminopenicillanic acid, and stir evenly; then add dropwise 48% hydrogen bromide aqueous solution (188kg) and 25% sodium chloride to the reactor Sodium nitrate solution (153kg), after dripping, the temperature was lowered to -10°C and reacted for 4 hours. The plate was monitored until the reaction was over. The organic phase was washed with water to neutrality to obtain 6-bromopenicillanic acid solution, and the obtained 6- The bromopenic acid solution is transferred to the oxidation reactor;
[0040] 2) Add 55kg of potassium bicarbonate to the oxidation reactor and stir for 1.5 hours, then add 102kg of diphenylmethyl chloride and 1kg of tetrabutylammonium bromide, heat to 30°C, stir and react for 3 hours, and detect the end point by thin layer chromatography When the benzhydryl chloride reaction is complete, add 0.5kg of sodium tungstate to the oxidation reaction kettle, an...
Example Embodiment
[0042] Example 2
[0043] 1) Add 500L of dichloromethane, 180kg of water to a 1500L reactor, add 120kg of 6-aminopenicillanic acid, and stir evenly; then add 50% hydrogen bromide aqueous solution (89.01kg) and 50% to the reactor dropwise Sodium nitrite solution (37.95.kg), after dripping, the temperature is lowered to -5°C and reacted for 3 hours. The plate is monitored until the reaction is over. The organic phase is washed with water until it is neutral to obtain 6-bromopenicillanic acid solution. The 6-bromopenicillanic acid solution is transferred to the oxidation reactor;
[0044] 2) Add 60kg of potassium bicarbonate to the oxidation reactor and stir for 2 hours, then add 102kg of diphenylmethyl chloride and 1kg of tetrabutylammonium bromide, heat up to 20℃, stir and react for 4 hours, and detect the end point by thin layer chromatography , When the benzhydryl chloride reaction is complete, add 0.9kg sodium tungstate to the oxidation reaction kettle. After the temperature dro...
Example Embodiment
[0046] Example 3
[0047] 1). Add 500L of dichloromethane, 180kg of water to a 1500L reactor, add 120kg of 6-aminopenicillanic acid, and stir evenly; then add dropwise 50% hydrogen bromide aqueous solution (267kg) and 60% sodium chloride to the reactor Sodium nitrate solution (94.875kg), after the dropwise addition, the temperature was lowered to 0°C and reacted for 2 hours. The plate was monitored until the reaction was over. The organic phase was washed with water to neutrality to obtain 6-bromopenicillanic acid solution, and the obtained 6 The bromopenic acid solution is transferred to the oxidation reactor;
[0048] 2) Add 50kg of potassium bicarbonate to the oxidation reactor and stir for 1 hour, then add 102kg of diphenylmethyl chloride and 1.1kg of tetrabutylammonium bromide, heat to 30℃, stir and react for 3 hours, and detect by thin layer chromatography At the end point, when the benzhydryl chloride reaction is complete, add 0.5kg of sodium tungstate to the oxidation reac...
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