Preparation method for synthesizing anidulafungin intermittent ([1,1':4',1''-Terphenyl]-4-carboxylic acid, 4''-(pentyloxy)-) through one-step method
A technology for p-pentyloxyterphenylcarboxylic acid and anidungin, which is applied in the field of preparation of p-pentyloxyterphenylcarboxylic acid, an intermediate for synthesizing anidungin by one-step method, can solve the problems of high production risk, low production cost, The problem of high production cost, to achieve the effect of low production cost, less three wastes, and short preparation route
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Embodiment 1
[0032] Add 30L of N,N-dimethylformamide to the prepared potassium carbonate solution (7600g potassium carbonate + 30L water) at room temperature, and then add 2000g of 4-bromobenzoic acid and 3650g of 1,4-benzenedi Pinacol borate. The system was replaced with nitrogen for 3 times, and 100 g of tetrakis(triphenylphosphine)palladium was added as a catalyst. Under the protection of nitrogen, the temperature was slowly raised to 73°C and stirred for 7 hours. Keeping the temperature constant, 2450 g of 4-n-pentyloxybromobenzene and 5 L of dimethylformamide solution were slowly added dropwise. After 4 hours of dropping, the reaction was continued for 8 hours. After the completion of the reaction, cool to 8°C, add 0.5N dilute hydrochloric acid aqueous solution to the system dropwise under stirring until the system pH=5, and stir for 2 hours after the addition. Suction filtration, the filter cake was rinsed twice with water and once with ethanol to obtain the target product anifungin...
Embodiment 2
[0034] Add 40L of N,N-dimethylformamide to the prepared sodium carbonate solution (5000g sodium carbonate + 25L water) at room temperature, and then add 1600g of 4-bromobenzoic acid and 3000g of 1,4-benzenedi Pinacol borate. The system was replaced with nitrogen for 3 times, and 95 g of [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride was added as a catalyst. Under the protection of nitrogen, the temperature was slowly raised to 76°C and stirred for 7 hours. Keeping the temperature constant, 1950 g of 4-n-pentyloxybromobenzene and 4.7 L of dimethylformamide solution were slowly added dropwise. After 3.5 hours of completion of the dropwise addition, the reaction was continued for 8 hours. After the reaction was completed, cool to 8° C. with a water bath, add 0.5 M dilute hydrochloric acid aqueous solution to the system dropwise with stirring until the system pH=4, and stir for 2 h after the addition. Suction filtration, the filter cake was rinsed twice with water and...
Embodiment 3
[0036] Add 20L of N,N-dimethylformamide to the prepared cesium carbonate solution (8600g cesium carbonate + 20L water) at room temperature, and then add 1000g of 4-bromobenzoic acid and 1800g of 1,4-benzenedi Pinacol borate. The system was replaced with nitrogen for 3 times, and 40 g of palladium acetate was added as a catalyst. Under the protection of nitrogen, the temperature was slowly raised to 75°C and stirred for 7 hours. Keeping the temperature constant, 1220 g of 4-n-pentyloxybromobenzene and 3 L of dimethylformamide solution were slowly added dropwise. After 2 hours of dropwise addition, the reaction was continued for 8 hours. After the reaction was completed, cool to 6° C. with a water bath, add 0.5 M dilute hydrochloric acid aqueous solution to the system dropwise with stirring until the system pH=5, and stir for 2 h after the addition. Suction filtration, the filter cake was rinsed twice with water and once with ethanol to obtain the target product anifungin inter...
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