Method for preparing ampicillin sodium
A technology for ampicillin sodium and ampicillin, applied in the field of compound preparation, can solve the problems of increasing manufacturing cost and environmental protection pressure, increasing the difficulty of solvent recovery, and low content of active ingredients, avoiding difficulty in solvent recovery and omitting granulation. Process, the effect of high content of active ingredients
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Embodiment 1
[0025] a) Preparation of liquid sodium isooctanoate: first add 250L of purified water to the alkali preparation tank, weigh 75kg of sodium hydroxide and add, stir until dissolved. Calculate the amount of isooctanoic acid added according to the molar ratio of sodium hydroxide to 1:1.1, and draw the isooctanoic acid into the reaction tank. Stir the prepared sodium hydroxide solution and press it into the reaction tank with isooctanoic acid, control the pH between 6.5 and 7.5, and stir for 30 minutes.
[0026] Open the jacket steam valve, heating temperature 85 ~ 100 ℃, vacuum gauge pressure <-0.06MPa, steam out about 250L of water under reduced pressure, add 200L of n-butanol to the residual liquid and heat to carry out azeotropic water banding, and determine the end point of detection When the water content of the sodium isooctanoate solution is less than 1.25%, open cold brine to cool down to ≤35°C, add about 800L of dichloromethane, and dilute the sodium isooctanoate solution...
Embodiment 2
[0031] a) Preparation of liquid sodium isooctanoate: first add 250L of purified water to the alkali preparation tank, weigh 75kg of sodium hydroxide and add, stir until dissolved. Calculate the amount of isooctanoic acid according to the molar ratio of sodium hydroxide to 1:0.8, and pump the isooctanoic acid into the reaction tank. The prepared sodium hydroxide solution was stirred and pressed into the reaction tank with isooctanoic acid, and stirred for 60 minutes. Open the steam valve of the jacket, decompress and steam out about 200L of water, add 300L of isobutanol to the residual liquid and heat to carry out azeotropic water removal. When the water content of the sodium isooctanoate solution is determined to be <1.25% at the end of the test, add Isobutanol, diluted to a concentration of 50% sodium isooctanoate solution for later use.
[0032] b) Preparation of ampicillin amine salt: take 100kg of ampicillin, according to the molar ratio of ampicillin and diisopropylamine...
Embodiment 3
[0036] a) Preparation of liquid sodium isooctanoate: first add 250L of purified water to the alkali preparation tank, weigh 75kg of sodium hydroxide and add, stir until dissolved. Calculate the amount of isooctanoic acid according to the molar ratio of sodium hydroxide to 1:1.3, and pump the isooctanoic acid into the reaction tank. The prepared sodium hydroxide solution was stirred and pressed into the reaction tank with isooctanoic acid, and stirred for 60 minutes. Evaporate about 250L of water under reduced pressure. After cooling down to about 25°C, add dichloromethane and dilute to 15% sodium isooctanoate solution for later use.
[0037]b) Preparation of ampicillin amine salt: take 100kg of ampicillin, according to the molar ratio of ampicillin and diisopropylamine is 1: 3.0, take diisopropylamine; Ampicillin is dissolved in 1000L methylene chloride to make ampicillin Penicillin organic solution; add 40kg of anhydrous magnesium sulfate, dehydrate the ampicillin organic so...
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