1,2-Ethanediamine, N1,N2-bis(phenylmethyl)-, acetate (1:2)

S3, adding the organic phase of the compound C and the toluene mixture obtained in the step S2 to a three-necked flask and distilling the mixture to a fraction without distillation.Then, it was cooled to 30 ° C, dissolved in 200 g of ethyl acetate, and heated to 60 ° C, followed by dropwise addition of 20 g of glacial acetic acid.The concentration of glacial acetic acid was 98percent, and the reaction was kept for 1.0 hour after the completion of the dropwise addition;Then slowly cool down to 5 ° C, 49.5 g of dibenzyl ethylenediamine diacetate wet product (ie, compound D containing water) was obtained by filtration.Drying at a temperature of 45 ° C finally gave 49.0 g of dibenzylethylenediamine diacetate (i.e., Compound D).S3, adding the organic phase of the compound C and the toluene mixture obtained in the step S2 to a three-necked flask and distilling the mixture to a fraction without distillation.Then, it was cooled to 30 C, dissolved in 200 g of ethyl acetate, and heated to 60 C, followed by dropwise addition of 20 g of glacial acetic acid.The concentration of glacial acetic acid was 98%, and the reaction was kept for 1.0 hour after the completion of the dropwise addition;Then slowly cool down to 5 C, 49.5 g of dibenzyl ethylenediamine diacetate wet product (ie, compound D containing water) was obtained by filtration.Drying at a temperature of 45 C finally gave 49.0 g of dibenzylethylenediamine diacetate (i.e., Compound D).[0033] About 20.4 g of a 20% aqueous solution of sodium hydroxide was added dropwise, Dropping time of about 6 ~ 8h, Drop finished, Stirring reaction 1 ~ 2h, To obtain a hydrolyzate solution, (HPLC detection of methoxy matter Reaction completed20% aqueous solution of acetic acid was added dropwise to about 10 to 15 mL, Adjust the pH to 6.0 ~ 7.0. Temperature control is less than 20 , The methanol was removed by distillation under reduced pressure, 200 g of ethyl acetate was added, 18.4 g (0.051 mol) of N, N'-dibenzylethylenediamine diacetic acid (benzyne salt) was added at a temperature of 20 to 30 C, Precipitation of a large number of solid after cooling to 0 ~ 5 , Continue stirring for 2h. filter, The filter cake was beaten with 150 mL of acetone for 10 minutes, filter, The filter cake was dried in vacuo at 50 C to give 45.8 g of a white solid (methoxy-cephalotin benzathine) The yield was 115.7% HPLC purity was 95.6% The melting point of 120.2 ~ 121.6In a stirred flask, 100 g of 3-Desacetyl Cephalothin, 1000 ml of dichloromethane, 100 ml of methanol and 100 ml of tetrahydrofuran were added, stirred and dissolved, cooled to -85 C with liquid nitrogen. A good solution of sodium methoxide(90 g sodium methoxide + 200 ml dichloromethane + 200 ml methanol) was added drop wise at a controlled temperature of -83 to -87 C. after the completion of addition added 35g of t-butyl hypochlorite and after the addition continue the reaction for 1 hour. 100 ml of a 50% glacial acetic acid solution was added and stirred for 15 minutes and raised temperature to -50 C. then 300 ml of 5% sodium chloride solution was added , heated to 0 ~ 5 C, stirred for 10 minutes and allowed to stand to separate the layers. The aqueous phase was extracted once with 100ml of dichloromethane , combined organic phase then decolored by adding activated charcoal. The filtration was carried out, then in filtrate added with 500 ml of water, stirred, and the mixture was adjusted to pH 7.2 to 7.5 with saturated sodium carbonate solution. After stirring for 10 minutes, the phases were separated and the temperature was raised to 30 C, benzathine diacetate was added with stirring for 1 hour, filtered and washed with a small amount of deionized water and dried to give 112 g of product, Weight Yield 112% (Description: The yield here is the weight yield, can be more than 100%, will not affect the purity).(2) Water 130.4ml, 146.4ml of methanol was added to a three neck reaction flask, cooled, compound IV410g, cooling. Slowly prechilled 4mol / L aqueous sodium hydroxidesolution to adjust PH 10, stir until complete reaction. Adjusted with acetic acid PH, temperature adjusting PH, temperature was raised to 25 , ethyl acetate was added, benzathine acetate 16g, 25 maintaining the reaction was stirred 2h. Filter cake was washed successively with water. Ethylacetate, and dried to give compound V287.11g (yield96%, purity 97.63%).In the flask, 130 ml of deionized water and 160 ml of methanol were added, and the mixture was stirred and lowered to -25 C, and 7 g of 7-a-methoxy cefotaxime cyclohexylamine salt was added.Slowly add 55ml of 10% sodium hydroxide solution, control the temperature -25 C, After the stirring reaction was completed for 60 min, 10 ml of 80% acetic acid was added, and the temperature was raised to 0 C.Add 80% acetic acid dropwise to control pH=6.5. Add sodium pyrosulfate 0.4g, 3g of activated carbon, kept at 0 C for 20 minutes, filtered, The activated carbon was washed with a 50% aqueous methanol solution, and the filtrate was combined.Concentration was stopped when concentrated to 190 ml in vacuo at 35 C. Temperature 30 C, Add 40 ml of ethyl acetate, Slowly add the prepared benzathine diacetate solution(Benzathine diacetate 15g + 140 ml of deionized water)After the addition is completed, the mixture is kept at 35 C and stirred for 90 minutes.The temperature was lowered to 0 C, stirred under heating for 2 h, filtered, and the filter cake was washed with 50 mL of acetone.Dry at 45 C, vacuum, 7-a-Methoxy-3-deacetyl cefotaxime benzathine salt was obtained in a yield of 0.94.(1) according to the ratio of organic solvent and water (1-3): 1 preparation of aqueous solution of organic solvent, and in condensation tank, opening stirring and jacket cooling water, to/99-210 g adding an aqueous solution of organic solvent per liter 6-aminopenicillanic acid; when the temperature dropped to 16 C the following, is added in the beginning to a concentration of 12% of NaOH solution, keeping PH value is 8-9, the 6-aminopenicillanic acid is dissolved; (2) according to the 6-aminopenicillanic acid with O-chlorobenzene a isooxazo acyl chloride in a molar ratio of 1 the [...] (0.95-1.15) that the proportion of the consecutive fins that fetches paradichlorbenzene a isooxazo acyl chloride, when the above-mentioned (1) step in the temperature of the sodium-salt solution is cooled to 10 C the following, is added in the beginning to the weighed O-chlorobenzene a isooxazo acyl chloride, is then started by adding the concentration of 13% NaOH solution of, and control of the tank value PH 6-8, the temperature does not exceed 26 C, until the value stable PH 6.5 and clarification reaction solution; (3) the above-mentioned (2) in the reaction liquid to clarify the sterile room through a sterilizing filter into the crystallization tank; (4) to the theoretical amount of compounding tank N, N-dibenzyl ethylene diamine diacetate, and control the diluted so that the concentration of 0.4-0.5g/ml, and the hot water heating jacket for N, N-dibenzyl ethylene diamine diacetate dissolved, then is put into the active carbon to stir, to decolourizations and absorbing impurity; N sample, N-dibenzyl ethylene diamine diacetate content, through a sterilizing filter into the room, for use; (5) the crystallization tank the water jacket for the feed liquid temperature reaches 10-40C, opening stirring, then slowly to the tank, even adding N, N-dibenzyl ethylene diamine diacetate solution, and then continuing to stir for 30 minutes; (6) open the crystallization tank discharge valve, the crystallization is the feed liquid into the oil pot, open at the same time vacuum filtration, wet filter cake to be pumped; the filter cake is washed with the above-mentioned (1) aqueous solution of the organic solvent in the step of washing three times, each time for washing 40L aqueous solution of organic solvent, and the concentration of the aqueous solution of an organic solvent for 30-100%, shall be a thickener; (7) the wet powder siebtechnik, the transferred to the double-cone dryer, open double-cone clamping set of steam-valve, controlling the drying temperature is 80 ±5 C, vacuum drying to moisture content is lower than 5%. Process for synthesizing austrastaph, without further processing, the process is simple, accurate data is easy to measure, the process flow is easy to implemen

Molecular Weight:360.4
Hydrogen Bond Donor Count:4
Hydrogen Bond Acceptor Count:6
Rotatable Bond Count:7
Exact Mass:360.20490738
Monoisotopic Mass:360.20490738
Topological Polar Surface Area:98.7
Heavy Atom Count:26
Complexity:202
Covalently-Bonded Unit Count:3
Compound Is Canonicalized:Yes