Preparation method for flucloxacillin sodium
A technology of flucloxacillin sodium and fluorophenyl, applied in the field of compound preparation, can solve the problems of high residual solvent, high production cost, long process route and the like, and achieve the effects of eliminating visible foreign matter, reducing production cost and short process route
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Embodiment 1
[0024] Add 10g of 6-APA into 40ml of water, cool down in an ice bath, adjust the pH to 7.0-9.0 with ammonia water, and add 10ml of acetone to make solution A;
[0025] Add 13.5g of 3-(2-chloro-6-fluorophenyl)-5-methylisoxazole-4-carbonyl chloride into 67.5ml of ethyl acetate to prepare solution B;
[0026] Add solution B to solution A, control the temperature of the system at -5°C to 10°C, adjust the pH of the reaction solution to 5.5-7.5 with ammonia water, and measure the content of flucloxacillin sodium in the solution by liquid phase detection to be 0.14g / ml, and the acylation reaction is completed ;
[0027] Add hydrochloric acid to adjust the pH of the system to 1.8-2.8, add ethyl acetate solution for extraction, then separate the liquid, discard the water phase, control the temperature of the organic phase at 25 ° C, add sodium isooctanoate DMF (di Methylformamide) solution 30ml, carry out salt-forming reaction, when the crystals precipitate, grow the crystals for 30 m...
Embodiment 2
[0030] Add 10g of 6-APA into 100ml of water, cool down in an ice bath, adjust the pH to 7.0-9.0 with sodium hydroxide, and add 30ml of acetone to make solution A;
[0031] Add 15 g of 3-(2-chloro-6-fluorophenyl)-5-methylisoxazole-4-carbonyl chloride to 100 ml of acetone to prepare solution B.
[0032] Add solution B to solution A, control the temperature of the system at -5°C to 10°C, adjust the pH of the reaction solution to 5.5-7.5 with sodium hydroxide, and carry out the acylation reaction. The content of flucloxacillin sodium in the solution is 0.085g by liquid phase detection / ml, the acylation reaction ends;
[0033] Add hydrochloric acid to adjust the pH of the system to 1.8-2.8, add n-butyl acetate to extract, then separate the liquid, discard the water phase, and control the temperature of the organic phase to 25°C; add 30ml of ethyl acetate solution of 11g sodium isooctanoate to form a salt Reaction, when the crystals are precipitated, grow the crystals for 30 minut...
Embodiment 3
[0036] Add 10g of 6-APA into 75ml of water, cool down in an ice bath, adjust the pH to 7.0-9.0 with sodium carbonate, and add 150ml of acetone to make solution A;
[0037] Add 16g of 3-(2-chloro-6-fluorophenyl)-5-methylisoxazole-4-carbonyl chloride into 150ml of acetone to prepare solution B;
[0038] Add solution B to solution A, control the temperature of the system at -5°C to 10°C, adjust the pH of the reaction solution to 5.5-7.5 with sodium carbonate, and carry out the acylation reaction. The content of flucloxacillin sodium in the liquid phase detection solution is 0.055g / ml, the acylation reaction ends;
[0039]Add hydrochloric acid to adjust the pH of the system to 1.8-2.8, add dichloromethane solution for extraction, then separate the liquids, discard the water phase, and control the temperature of the organic phase at 25°C; add 12g of sodium isooctanoate to methyl isobutyl ketone (MIBK) Solution 60ml, carry out salt formation reaction, when crystals are precipitate...
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