Preparation method of milbemycin oxime
A technology of milbemycin and milbemycin, applied in the direction of organic chemistry, can solve the problems of high cost, large investment in equipment, and difficulty in realizing industrialized production, and achieve the effect of increasing production capacity and reducing costs
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Embodiment 1
[0018] The preparation method of the milbemycin provided by the present embodiment, its steps are as follows: 1, take by weighing 130Kg dried milbemycelium, milbemycin A 3 and A 4 The calibrated contents are 0.55% and 2.57%, respectively, which are added to a 1500L stirring extraction tank, and 750L of n-heptane and acetone mixed solvent with a volume ratio of 6:1 are added, stirred and extracted at 30rpm for 2h, filtered, and the filter cake is subjected to the above conditions Extract 2 times and combine the filtrates. Pump the filtrate into the concentrator, concentrate under reduced pressure at 55°C to about 300L, and obtain concentrate A.
[0019] 2. Transfer the concentrated solution A from the previous step to a 1000L extraction kettle, add 300L of 85% ethanol aqueous solution, stir at 25rpm for 15min, let it stand for 30min, and separate the liquids. The upper n-heptane phase is extracted once again with 300L of 85% ethanol solution, and the extracts are combined , c...
Embodiment 2
[0025] The preparation method of the milbemycin provided by the present embodiment, its steps are as follows: 1, take by weighing 130Kg dried milbemycelium, milbemycin A 3 and A 4 The calibrated contents are 0.56% and 2.59%, respectively, which are added to a 1500L stirring extraction tank, and 950L of n-heptane and acetone mixed solvent with a volume ratio of 4:1 are added, stirred and extracted at 30rpm for 2h, filtered, and the filter cake is subjected to the above conditions Extracted 4 times and combined the filtrates. Pump the filtrate into the concentrator, concentrate under reduced pressure at 50°C to about 300L, and obtain concentrate A.
[0026] 2. Transfer the concentrated solution A from the previous step to a 1000L extraction kettle, add 290L of 76% ethanol aqueous solution, stir at 25rpm for 15min, let stand for 30min, separate the liquids, extract the upper n-heptane phase with 300L85% ethanol solution once again, and combine the extracts , concentrated under ...
Embodiment 3
[0032] The preparation method of the milbemycin provided by the present embodiment, its steps are as follows: 1, take by weighing 130Kg dried milbemycelium, milbemycin A 3 and A 4 The calibrated contents are 0.58% and 2.55%, respectively, which are added to a 1500L stirring extraction tank, and 1200L of n-heptane and acetone mixed solvent with a volume ratio of 8:1 are added, stirred and extracted at 30rpm for 2h, filtered, and the filter cake is subjected to the above conditions Extracted 3 times and combined the filtrates. Pump the filtrate into the concentrator, concentrate under reduced pressure at 60°C to about 300L, and obtain concentrate A.
[0033] 2. Transfer the concentrated solution A from the previous step to a 1000L extraction kettle, add 250L of 88% ethanol aqueous solution, stir at 25rpm for 15min, let it stand for 30min, and separate the liquids. The upper n-heptane phase is extracted once again with 300L of 85% ethanol solution, and the extracts are combined ...
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