CN101693654A

CN101693654A - Method for refining aloe-emodin by reagent-grade N, N-dimethyl acetamide

Info

Publication number: CN101693654A
Application number: CN200910035514A
Authority: CN
Inventors: 黄再新
Original assignee: Individual
Current assignee: Individual
Priority date: 2009-09-23
Filing date: 2009-09-23
Publication date: 2010-04-14

Abstract

The invention relates to a method for refining aloe-emodin by reagent-grade N, N-dimethyl acetamide, belonging to the technical field of medicament production. The method comprises the following process steps: dissolving crude aloe-emodin in reagent-grade N,N-dimethyl acetamide; wherein reagent-grade acetic acid with the volume ratio of 1 percent is added in the reagent-grade N, N-dimethyl acetamidein; forming a saturated solution at the high temperature of 100-105 DEG C; adding active carbon to destaining for 0.5-1.0h; filtering and reducing the temperature to 0-3 DEG C to separate out aloe-emodin crystals; and drying to obtain an aloe-emodin competitive product. A solvent with larger solubility to aloe-emodin is found in the invention, and rheic acid is refined by dissolving the aloe-emodin in the solvent by utilizing a conventional chemical refining method. The method is simple, convenient and feasible, greatly improves the yield and lowers the energy consumption.

Description

The method of SILVER REAGENT N,N-dimethylacetamide refining aloe-emodin

(1) technical field

The present invention relates to a kind of process for purification of rhabarberone.Belong to technical field of medicament.

(2) background technology

Rhabarberone is the monomer of anthraquinone derivative, has, and is considered to have the medicine of many target spots function, anti-tumor activity, P388 leukemia cell is had restraining effect; Have anti-microbial activity, staphylococcus, suis, diphtheria corynebacterium, Bacillus subtilus, anthrax, paratyphosum Bacterium, dysentery bacterium etc. are all had restraining effect; Have immunosuppressive action, can suppress organism antibody and produce; Have discharge function, human body is had activity under stronger the rushing down, constipation and hemorrhoid are had special efficacy; Has functions of lowering blood-fat and reducing weight; Has the hair soft of making and glossy, the easily effect of pleasant, anti-dandruff; Can protect teak to avoid the invasion and attack of termite.Obtain abroad at present widely applying, simultaneously its---diacetyl rhein (diacerein), antitumor good medicine---main raw material of rhubarb yellow, daunomycin, Zorubicin of still treating the good medicine of osteoarthropathy.This product is very wide in the market outlook of American-European countries, also begins at home to be applied.

Rhabarberone generally all extracts from natural rheum officinale etc. and obtains, to this existing patent report (CN03153223.3, CN200610017742.0).Existing in addition unit begins to obtain rhabarberone (CN200580038713.6) by synthetic route in producing the rhubarb yellow process.No matter extraction method or synthesis method, purification step or employing high-speed countercurrent chromatography to product perhaps adopt the chromatography column method, perhaps adopt recrystallization method.For the former two, there is the defective that facility investment is big, actually operating is inconvenient; For recrystallization method, though rhabarberone dissolves in acetaldehyde, benzene, ethyl acetate, hot ethanol, weak ammonia, yellow soda ash and aqueous sodium hydroxide solution, then foreign matter content is big, purification effect is not good but extract after the dissolving in basic solution again, then there is solubleness problem on the low side in all the other organic solvents, limited the raising of unit output, energy consumption is bigger than normal.For example rhabarberone only dissolves 5 milligrams in 1000 milliliters 78 ℃ (boiling point) hot ethanols, only dissolves 8～9 milligrams in 1000 milliliters of 100 ℃ of left and right sides hot toluenes.

(3) summary of the invention

The objective of the invention is to overcome rhabarberone and have solubleness problem on the low side, the method for a kind of rhabarberone at the higher SILVER REAGENT N,N-dimethylacetamide refining aloe-emodin of organic solvent dissolution degree is provided at organic solvent.

The objective of the invention is to be achieved through the following technical solutions: by the chemical refining method of routine, crude product rhabarberone (HPLC content 70～90%) is dissolved in SILVER REAGENT N, N-N,N-DIMETHYLACETAMIDE (the SILVER REAGENT acetic acid that wherein adds 1% volume ratio, prevent the rhabarberone alienation), forming saturated solution (hot N under 1000 milliliters of these temperature under 100～105 ℃ of high temperature, 240～245 milligrams of rhabarberones of solubilized in the N-N,N-DIMETHYLACETAMIDE), added activated carbon decolorizing 0.5～1.0 hour, be cooled to 0～3 ℃ after the filtration, promptly separate out orange rhabarberone crystal (fine acicular), oven dry (preferably vacuum-drying, so that the N,N-dimethylacetamide removal of solvents is thorough) after promptly obtain rhabarberone elaboration (HPLC content 85～98% even higher).

The invention has the beneficial effects as follows:

The present invention has found a kind of solvent bigger to rhabarberone solubleness, and by the chemical refining method of routine, the method that rhabarberone is dissolved in this solvent is made with extra care rhubarb yellow, and is simple and easy to do, greatly improved output, reduced energy consumption.

(4) embodiment

Be illustrated with specific embodiment below:

1,260 gram rhabarberone crude products (HPLC content 90.6%) is dropped into the 1000ml flask, the SILVER REAGENT N that adds 900mlL, the SILVER REAGENT acetic acid of N-N,N-DIMETHYLACETAMIDE and 9ml stirs, and heats to 100～105 ℃ and keeps this temperature rhabarberone fully to be dissolved in 0.5 hour.

2, in above-mentioned flask, add 5 gram gacs, continue to keep 108～110 ℃ 0.5～1 hour.

3, carry out suction filtration with B after aforesaid liquid being filtered postcooling to 0～3 ℃, filter cake is with the N,N-dimethylacetamide flushing of 100ml three times.

4, filtration cakes torrefaction (vacuum-drying, 80～85 ℃ of temperature) is pulverized rhabarberone 203 grams (HPLC content 98.2%) that promptly obtain behind the purifying after 2 hours.

Claims

1. SILVER REAGENT N, the method of N-N,N-DIMETHYLACETAMIDE refining aloe-emodin, it is characterized in that described method comprises following technological process: the crude product rhabarberone is dissolved in SILVER REAGENT N, the N-N,N-DIMETHYLACETAMIDE, described SILVER REAGENT N, the N-N,N-DIMETHYLACETAMIDE adds the SILVER REAGENT acetic acid that 1% volume ratio is arranged, under 100～105 ℃ of high temperature, form saturated solution, added activated carbon decolorizing 0.5～1.0 hour, be cooled to 0～3 ℃ after the filtration, promptly separate out the rhabarberone crystal, promptly obtain the rhabarberone elaboration after the oven dry.