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Method for recovering lovastatin from lovastatin crystallization mother liquor

A technology of lovastatin and crystallization mother liquor, which is applied in the field of lovastatin production technology, can solve the problems of lengthy and complicated operation process, high safety and environmental protection pressure, and high solvent consumption, and achieve simple operation steps, improved recovery rate, and accelerated recovery process Effect

Inactive Publication Date: 2016-10-19
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The above methods all involve the process of cyclization after the ring-opening treatment of the crystallization mother liquor. The operation process is lengthy and complicated, and there are many operation steps involving equipment, and a large number of Macroporous resins, a large amount of organic solvents such as ethyl acetate, high solvent consumption in the recycling process, and high pressure on safety and environmental protection

Method used

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  • Method for recovering lovastatin from lovastatin crystallization mother liquor

Examples

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Comparison scheme
Effect test

Embodiment 1

[0111] Take 1000ml of lovastatin crystallization mother liquor, wherein the lovastatin unit is 54666U / ml, add 400ml of 0.4mol / L sodium bicarbonate solution, stir and wash for 30 minutes, after stirring and washing is completed, let stand, separate the water phase, and obtain the organic phase 975ml; add 400ml of 0.4mol / L sodium bicarbonate solution to the organic phase, stir and wash for 30 minutes, let it stand, separate the water phase, and obtain 965ml of the organic phase; add 965ml of 1% (w / v, that is, dissolve 1g of oxalic acid in 100ml of water to configure 1% oxalic acid aqueous solution, the same below) was stirred and washed for 1 hour, left to stand, and the aqueous phase was separated to obtain 963 ml of organic phase. Add 100ml of 2% oxalic acid ethanol solution (2g of oxalic acid in 100ml of absolute ethanol) to the washed organic phase for cyclization treatment at 80°C for 2 hours, then properly concentrate at 73°C and vacuum degree ≤ -0.09Mpa , after standing f...

Embodiment 2

[0113] Take 2000ml of lovastatin crystallization mother liquor, wherein the unit of lovastatin is 54696U / ml, add 750ml of 0.4mol / L sodium bicarbonate solution and stir and wash for 30 minutes, after stirring and washing is completed, let stand, separate the water phase to obtain the organic phase 1980ml; add 1980ml of 1% oxalic acid aqueous solution, stir and wash for 1 hour, let stand, separate the water phase, and obtain 1960ml of the organic phase. Add 58.8ml of glacial acetic acid to the washed organic phase, cyclize at 80°C for 2 hours, concentrate properly at 75°C, vacuum degree ≤ -0.09Mpa, stand for crystallization for 8 hours, and filter with suction to obtain lovastatin The crude product is 87.8g, the content is 73.2%, and the yield is 80.26%.

Embodiment 3

[0115] Take 1000ml of lovastatin crystallization mother liquor, wherein the lovastatin unit is 50696U / ml, add 300ml of 0.4mol / L sodium bicarbonate solution, stir and wash for 30 minutes, after stirring and washing is completed, let stand, separate the water phase, and obtain the organic phase 980ml; add 980ml of 1% oxalic acid aqueous solution, stir and wash for 1 hour, let stand, separate the water phase, and obtain 965ml of the organic phase. Add 9.7ml of acetic acid to the washed organic phase, cyclize at 80°C for 2 hours, concentrate properly at 75°C under vacuum ≤ -0.09Mpa, stand for crystallization for 8 hours, and filter with suction to obtain Loval The crude statin was 39.62g, the content was 73.8%, and the yield was 78.15%.

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Abstract

The invention provides a method for recovering lovastatin from lovastatin crystallization mother liquor. The method comprises the following steps: (1) mixing the lovastatin crystallization mother liquor with an alkaline aqueous solution to perform washing, and separating the lovastatin crystallization mother liquor from the alkaline aqueous solution to obtain an organic phase; (2) mixing the organic phase obtained in the step (1) with an acid aqueous solution to perform washing, and separating the organic phase from the acid aqueous solution to obtain an organic phase; (3) performing a cyclization reaction on the organic phase obtained in the step (2); and (4) concentrating the cyclized organic phase obtained in the step (3), and crystalizing the concentrated organic phase to obtain the lovastatin. The method is simple in operating steps, safer, more environmentally friendly, and suitable for industrial continuous production. The product recovery rate of the mother liquor is increased, and solvent consumption in a recovery process is lowered. Moreover, the requirement of a recovery production condition on equipment is low, and the recovery progress in production can be accelerated.

Description

technical field [0001] The invention relates to the field of lovastatin production technology, in particular to a method for recovering lovastatin from lovastatin crystallization mother liquor. Background technique [0002] Lovastatin is a cholesterol-lowering drug derived from microbial hydroxymethylglutaryl-CoA reductase inhibitors. Because of its clear mechanism of action and remarkable clinical efficacy, it is currently an important clinical treatment for cardiovascular and cerebrovascular diseases (such as atherosclerosis and coronary heart disease) drugs. Lovastatin is a secondary metabolite of fungi, and the main industrial bacteria producing it are Aspergillus terreus, Penicillium citrinum and Monascus ruber. [0003] The chemical name of lovastatin is: (S)-2-methylbutanoic acid-(1S,3R,7S,8S,8aR)-1,2,3,7,8,8a-6H-3,7-di Methyl-8-(2-((2R,4R)-4-hydroxy-6-oxo-2H-tetrahydropyranyl)-ethyl)-1-naphthyl ester. The molecular formula of lovastatin is C 24 h 36 o 5 , the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/30
CPCC07D309/30
Inventor 詹付凤张洪兰何新亮张新许
Owner NEW FOUNDER HLDG DEV LLC
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