Preparation method of sodium salt of pravastatin

A technology of naveladine sodium and naveladine, which is applied to the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., and can solve the problems of unhealthy operators, extremely high equipment production environment requirements, and increased investment and energy consumption issues

A technology of naveladine sodium and naveladine, which is applied to the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., and can solve the problems of unhealthy operators, extremely high equipment production environment requirements, and increased investment and energy consumption issues

CN101580466AActive Publication Date: 2009-11-18SHANGHAI TECHWELL BIOPHARMACEUTICALS CO LTD
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  • Preparation method of sodium salt of pravastatin
  • Preparation method of sodium salt of pravastatin
  • Preparation method of sodium salt of pravastatin

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preparation example Construction

[0043] In another preference of the present invention, the preparation method of described naveladine sodium comprises the following steps:

[0044](a) Naveladidine salt is transferred to the first solvent by extraction to form an organic solution containing naveladine; the first solvent is selected from one or more of the following groups: methyl formate, formic acid n-propyl, isopropyl formate, n-butyl formate, methyl acetate, ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, sec-butyl acetate, isobutyl acetate, tert-butyl acetate ester;

[0045] (b) adding an inorganic or organic base whose cation is a sodium ion to the organic solution obtained in step (a), to obtain a precipitate;

[0046] (c) Repeat the steps from (a) to (b) for the precipitate obtained in step (b) for 1-5 times to obtain naveladine sodium; preferably repeat 1-3 times.

[0047] In the present invention, the organic solution containing naveladidine can be obtained using methods famili...

Embodiment 1

[0071] 35 grams of naveladidine (purchased from Shanghai Tianwei Biopharmaceutical Co., Ltd.) was completely dissolved in 750 mL of ethyl acetate at 20 ° C, and then a methanol solution containing 1M NaOH was added thereto until the pH was above 7. 80 mL of methanol solution of 1M NaOH was collected by filtration and dried in vacuo to obtain 31 grams of white crystalline powder of naveladidine sodium.

[0072] The specific rotation of naveledadine sodium is +157°, the purity is 99.95%, and the content of the structural analogue 3α-naveledadine sodium is 0.03%.

Embodiment 2

[0074] 350 grams of naveladine sodium crude product was completely dissolved in 2L of water at 20°C, then 4L of ethyl acetate was added thereto, stirred, and washed with 0.5M H 2 SO 4 Adjust the pH below 4, statically discard the water phase, and then add an ethanol solution containing 1M NaOH to it until the pH is above 800mL, add a total of 800mL of an ethanol solution containing 1M NaOH, collect the precipitate by filtration, and dry it in vacuum to obtain the refined naphthalene Taiding sodium white crystalline powder 330 grams.

[0075] Its assay result and the comparative data with naveladine sodium crude product purity are as follows:

[0076]

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Abstract

The invention discloses a preparation method of sodium salt of pravastatin, which comprises the following steps: adding inorganic alkaline or organic alkaline containing sodium ions as positive ions into organic solution containing the pravastatin until pH is more than 7 and obtaining sodium pravastatin; the organic solution containing the pravastatin comprises the pravastatin and first solvent, wherein the first solvent is selected from one or a plurality of methyl formate, n-propyl formate, isopropyl formate, n-butyl formate, methyl acetate, ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, sec-butyl acetate, isobutyl acetate and tert-butyl acetate.

Description

technical field [0001] The present invention relates to the preparation method of the sodium salt of naveladine. Background technique [0002] Naveladine sodium (pravastatin sodium) is one of the statins, its chemical name is {1S-[1α(βs * , δs * ), 2α, 6α, 8β (R * ), 8aα]}-1,2,6,7,8,8a-hexahydro-β,δ,6-trihydroxy-2-methyl-8-(2-methyl-1-oxobutoxy) -1-naphthoyl heptanoic acid monosodium salt, which and lovastatin, simvastatin, atorvastatin, fluvastatin and their derivatives and analogues are hydroxymethylglutaryl coenzyme A (HMG-CoA) Reductase inhibitors are used in the treatment of hypercholesterolemia or atherosclerosis. [0003] [0004] The structural formula of naveladine sodium [0005] Naveladine sodium exerts its lipid-lowering effect from two aspects: first, it reversibly inhibits the activity of HMG-CoA reductase, blocks the biosynthesis of cholesterol in the liver, reduces the amount of cholesterol in cells to a certain extent, stimulates The compensatory in...

Claims

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Application Information

Patent Timeline
18 Nov 2009
Publication
CN101580466A
IPC
C07C69/013; C07C69/22; C07C67/48; C07C67/28; A61K31/22; A61P3/06; A61P9/10
Inventors
季晓铭; 姚勇