Method of preparing diacetyl parietic acid from rhubarb extract
A technology for diacetyl rhein and rhubarb extract, which is applied in the field of preparing diacetyl rhein, can solve the problems of difficult control of aloe-emodin, high cost industrialized production, long routes, etc., so as to improve the total product yield and reduce production costs. , the effect of low price
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Embodiment 1
[0021] (1) Add 2.1 grams of a mixture containing rhein, chrysophanol and aloe-emodin (4:5:1) into 38 milliliters of acetic anhydride, stir and place for 10 minutes;
[0022] (2) Add 2.1 g of anhydrous sodium acetate to the reaction solution, heat up to 95° C., stir and react for 90 minutes, filter while hot, cool to crystallize, filter and wash with water to obtain the diacetyl compound;
[0023] (3) The obtained diacetyl compound was added to 120 milliliters of glacial acetic acid-acetic anhydride (10:1) mixed solution, the temperature was raised to 50° C., and 64 milliliters of chromium trioxide solution (2.2 grams of chromium trioxide dissolved in 4 milliliter of deionized water, and then add 60 milliliters of glacial acetic acid), after the dropwise addition, keep it warm at 60-65°C for 3 hours, then pour the oxidized solution into ice water, a pale yellow precipitate precipitates, filters, washes with water, and dries to obtain Diacetylrhein crude product;
[0024] (4) A...
Embodiment 2
[0028] (1) Add 2.1 grams of a mixture containing rhein, chrysophanol and aloe-emodin (4:6:1) into 38 milliliters of acetic anhydride, stir and place for 10 minutes;
[0029] (2) Add 0.8 g of anhydrous potassium acetate to the reaction solution, heat up to 95° C., stir and react for 90 minutes, filter while hot, cool to crystallize, filter and wash with water to obtain the diacetyl compound;
[0030] (3) The obtained diacetyl compound was added to 120 milliliters of glacial acetic acid-acetic anhydride (10:1) mixed solution, the temperature was raised to 50° C., and 64 milliliters of chromium trioxide solution (2.2 grams of chromium trioxide dissolved in 4 milliliter of deionized water, and then add 60 milliliters of glacial acetic acid), after the dropwise addition, keep it warm at 60-65°C for 3 hours, then pour the oxidized solution into ice water, a pale yellow precipitate precipitates, filters, washes with water, and dries to obtain Diacetylrhein crude product;
[0031] (4...
Embodiment 3
[0034] (1) Add 2.8 grams of chrysophanol and aloe-emodin mixture (5:1) into 60 ml of acetic anhydride and pyridine mixture (10:1), react at 50°C for 2 hours, and pour the reactants into Put 150 ml of cold water in a stoppered cone, place the cone in an ice-water mixture to cool, crystallize, and separate out yellow crystals by suction filtration to obtain the diacetyl compound;
[0035] (2) Dissolve the diacetyl compound obtained in 120ml of glacial acetic acid-acetic anhydride mixture (10:1), and add dropwise 70ml of chromium trioxide solution (3.3g of chromium trioxide dissolved in 5ml of deionized water, then add glacial acetic acid (65 milliliters), add in about 30 minutes. After the addition, the temperature was raised to 60-65° C. to continue stirring for 4 hours, and then the dark green reaction solution was added to 800 ml of ice-cold deionized water containing disodium edetate for crystallization. After the product is completely precipitated, filter with suction, was...
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