Nemadectin purification method

A technology of nimoctin and purification method, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of difficulty in using nimoctin, low purity of nimoctin, high energy consumption, etc. , to achieve the effect of simple and easy method, low cost and low energy consumption

Active Publication Date: 2015-01-21
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The nemoctine obtained by this method has low purity and low efficiency, which brings difficulties for the use of nemoctine
[0007] Chinese patent application No.201010237843.5 discloses a method for preparing nemoctine, wherein the method includes: direct spray

Method used

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  • Nemadectin purification method

Examples

Experimental program
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Effect test

Embodiment 1

[0077] Preparation of diethylamine acetate: add 100ml of acetic acid into 180ml of diethylamine under stirring, set aside.

[0078] Adjust the pH of 10 L of nimoctine fermentation broth to 3.1 with dilute sulfuric acid, and filter to obtain 451.2 g of filter cake; add 1.5 L of isopropanol for extraction, filter to obtain a filtrate; concentrate and recover isopropanol. Add 0.6L of dichloromethane to the solid mixture, add 0.4L of 5% sodium bicarbonate solution, stir and wash for 1h, let stand to separate layers; take the upper layer, concentrate and recover the solvent to obtain 50.2g of crude product of nimoctine, the HPLC purity is 35.67% .

[0079] Add 200ml of diethylamine acetate to the obtained crude nemoctin, stir to dissolve, and filter; add 60ml of heptane to the filtrate for extraction, remove the lower layer, cool to -2~0°C, add 250ml of water dropwise under stirring, crystallize, filter, and use 15 % (v / v) isopropanol aqueous solution, and dried under reduced pres...

Embodiment 2

[0081] Preparation of triethylamine acetate: add 100ml of acetic acid into 243ml of triethylamine under stirring, set aside.

[0082] Adjust the pH of 10 L of nimoctine fermentation broth to 3.2 with dilute hydrochloric acid, and filter to obtain 463.5 g of filter cake; add 1.2 L of isopropanol for extraction, and filter to obtain a filtrate; concentrate to recover isopropanol. Add 0.5 L of dichloromethane to the solid mixture, add 0.35 L of 5% sodium bicarbonate solution, stir and wash for 1 h, let stand to separate layers; take the upper layer, concentrate and recover the solvent to obtain 52.4 g of crude product of nimoctine, the HPLC purity is 33.59% .

[0083]Add 220 ml of triethylamine acetate to the obtained crude nemoctin, stir to dissolve, and filter; add 70 ml of hexane to the filtrate for extraction, remove the lower layer, cool to -5-4°C, add 250 ml of water dropwise under stirring, crystallize, filter, and use 15 % (v / v) isopropanol aqueous solution, dried under ...

Embodiment 3

[0085] Preparation of diethylamine acetate: add 100ml of acetic acid into 180ml of diethylamine under stirring, set aside.

[0086] Adjust the pH of 10 L of nimoctine fermentation broth to 5.0 with phosphoric acid, and filter to obtain 475.6 g of filter cake; add 1.5 L of ethanol to extract, filter to obtain a filtrate; concentrate to recover ethanol. Add 0.6L of dichloromethane to the solid mixture, add 0.4L of 5% sodium bicarbonate solution, stir and wash for 1h, let it stand for stratification; take the upper layer, concentrate and recover the solvent to obtain 55.4g of crude product of nimoctine, the HPLC purity is 30.71% .

[0087] Add 200ml of diethylamine acetate to the obtained crude nemoctin, stir to dissolve, and filter; add 60ml of methylcyclohexane to the filtrate for extraction, remove the lower layer, cool to -1~0°C, add 250ml of water dropwise under stirring, crystallize, and filter , washed with 20% (v / v) aqueous ethanol, and dried under reduced pressure to ob...

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Abstract

The invention provides a nemadectin purification method. The method comprises the steps that: (1) a nemadectin crude product is provided; (2) the nemadectin crude product is mixed with liquid-state organic salt, and filtering is carried out, such that a filtrate is obtained; (3) the obtained filtrate is mixed with C5-C20 alkane, such that washing is carried out; and separation is carried out, such that a liquid-state organic salt-phase solution is obtained; and (4) the liquid-state organic salt-phase solution obtained in the step (3) is subjected to cooling crystallization, such that nemadectin is obtained. Compared with prior arts, the method has the following advantages: defects of current methods such as resin absorption separation are overcome; the purity of obtained nemadectin is high; the method is simple and feasible; energy consumption is low; cost is low; and single processing capacity is high. The method is suitable for industrialized mass productions.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a method for purifying nemoctine. Background technique [0002] Nemadectin is a sixteen-membered macrolide antibiotic produced by Streptomyces cyaneogriseus sp. Like mycin, it exhibits good antiparasitic activity. Nimoctine is white powder, soluble in methanol, ethanol, dichloromethane, dimethyl sulfoxide, formamide dimethylamide. Molecular formula of Nimoctin: C 36 h 52 o 8 , molecular weight: 312.3705, molecular formula as shown in formula I below: [0003] [0004] In the 1990s, the area under the control of agricultural diseases and insect pests in my country was 270 million ha 2 , 90% of the use of pesticides for prevention and control, reducing food loss of 31.5 billion catties; a large number of chemical pesticides have a great impact on the environment, and even caused serious pollution, endangering people's health. Nimoctine, as an antiparasitic antibiotic, ...

Claims

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Application Information

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IPC IPC(8): C07H19/01C07H1/06
CPCC07D493/22
Inventor 彭平郭萍张洪兰易钟
Owner NEW FOUNDER HLDG DEV LLC
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