Chemical synthesis method of 3,5-dichloro-4-hydroxy-2-methoxy-6-methyl-benzoic acid
A synthetic method, methoxy technology, applied in the field of chemical synthesis of drug metabolites, can solve the problems of unavailable chlamycin and julamycin, long reaction route, cumbersome reaction process, etc., and achieve low price , simple method and easy-to-obtain raw materials
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Embodiment 1
[0026] Put 32.12g of simexol premix (purchased from Eli Lilly and Company of the United States) into a 500mL conical flask, add 350mL ethyl acetate to the conical flask to soak, shake once every 1h, and suction filter after 8h , the filtrate was distilled under reduced pressure, and the recovered ethyl acetate was used again for the extraction of avilamycin, evaporated to dryness to obtain a light yellow solid, and the solid was put into a vacuum oven at 45°C to dry for 4 hours to obtain 4.51 g of avilamycin Vegetarian crude products.
[0027] Put 4.26g of the crude product of avelamycin into a three-necked flask equipped with a spherical condenser, put it in a water bath at 90°C, and stir it with 50mL of acetone-water mixed solution with a volume ratio of 3:1 until it dissolves, then suction filter while it is hot , the filtrate was slowly lowered to room temperature and then cooled to 4 ° C, left for 6 to 9 hours and then suction filtered, the filter cake was washed with abs...
Embodiment 2
[0031] Put 100.26g of Sumisu into a 1.5L Erlenmeyer flask, add 1100mL ethyl acetate to the Erlenmeyer flask for soaking, shake once every 1h, suction filter after 6h, distill the filtrate under reduced pressure, and use the recovered liquid again For the extraction of avelamycin, evaporate to dryness under reduced pressure to obtain a light yellow solid, put the solid in a vacuum oven at 45° C. and dry for 5 hours to obtain 12.65 g of crude product of avelamycin.
[0032] Put the crude product of 11.24g of avelamycin into a three-neck flask equipped with a spherical condenser, put it in a water bath at 90°C, stir it with 145mL of acetone-water mixed solution with a volume ratio of 3:1 until dissolved, and suction filter while it is hot , the filtrate was slowly lowered to room temperature and then cooled to 4°C, left to stand for 8 hours and then suction filtered, the filter cake was washed with absolute ethanol to obtain a recrystallized product of avelamycin, and the product ...
Embodiment 3
[0036] Put 202.58g of Sumisu into a 3L Erlenmeyer flask, add 2150mL of ethyl acetate to the Erlenmeyer flask to soak, shake once every 1h, suction filter after 7h, distill the filtrate under reduced pressure, and recover the ethyl acetate solution Used for re-extraction of avelamycin, evaporated to dryness to obtain a light yellow solid, and put the obtained solid in a vacuum oven at 45° C. for 6 hours to obtain 28.72 g of crude product of avelamycin.
[0037] Put 25.12g of crude product of avelamycin into a three-neck flask equipped with a spherical condenser, put it in a water bath at 90°C, stir it with 270mL of acetone-water mixed solution with a volume ratio of 3:1 until dissolved, and then suction filter while it is hot , the filtrate was slowly lowered to room temperature and then cooled to 4°C, left to stand for 6 hours and then filtered with suction, the filter cake was washed with absolute ethanol to obtain a recrystallized product of avelamycin once, and the product w...
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