Preparation method of 6,7-epoxy ligustilide
A technology of ligustilide and epoxy, which is applied in the field of preparation of chemical components of traditional Chinese medicine, can solve the problems of expensive raw materials, cumbersome steps, and difficulty in large-scale preparation, and achieves a simple and easy method, cheap and easy-to-obtain raw materials, and large-scale preparation. Effect
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Embodiment 1
[0026] A preparation method of 6,7-epoxyligustilide, the steps are:
[0027] (1) Reaction: Add 100ml of water-ethanol (25:75, v / v) and 5g of Ligusticum chuanxiong volatile oil (ligustilide content 19.5%, w / w) into a 250ml round-bottomed flask and stir for 5 minutes at room temperature. Take 10g of potassium peroxymonosulfate composite salt, slowly add it to the reaction system, stir at room temperature for 5 minutes, and then react in a water bath at 80°C. The reaction will be terminated when the ligustilide chromatographic peak area in the reaction solution decreases by 75% ;
[0028] (2) Detection: Waters Acquity UPLC chromatograph; column Waters BEH C18 (50mm×2.1mm, 1.7μm); mobile phase acetonitrile (A)-0.1% phosphoric acid water (B); gradient elution 0~0.5min (20 % A), 0.5~3.0min (20% A~70% A), 3.0-3.5min (70% A~100% A), 3.5~4.0min (100% A), 4.0~4.01min (100% A) ~20%A), 4.01~5.0min (20% A); flow rate 0.4ml / min; column temperature 35˚C; detection wavelength 280nm. The results...
Embodiment 2
[0032] A preparation method of 6,7-epoxyligustilide, the steps are:
[0033] (1) Preparation of angelica extract: 1kg of angelica medicinal materials, crushed, passed through No. 3 sieve, and extracted by steam distillation to obtain 5.7g angelica volatile oil;
[0034] (2) Reaction: 40 ml of water-1,4-dioxane (10:90, v / v) and 2 g of the volatile oil of angelica prepared in step (1) (liquitolide content 42.1%, w / w) Add them to a 100 ml round bottom flask one by one, and stir at room temperature for 5 minutes. Take 9 g of potassium permonosulfate composite salt, slowly add it to the reaction system, stir at room temperature for 5 minutes, and then react in a water bath at 100°C; the progress of the reaction is monitored by liquid chromatography, and the peak area of ligustilide in the reaction solution The reaction is terminated when it is reduced by 85%;
[0035] (3) Separation: After the reaction, the insoluble matter was removed by suction filtration, the filtrate was concentr...
Embodiment 3
[0037] A preparation method of 6,7-epoxyligustilide, the steps are:
[0038] Add 20 ml of water-methanol (5:95, v / v) and 0.5 g of crude ligustilide (content 80%, w / w) into a 50 ml round-bottom flask, and stir for 5 minutes at room temperature; 3 g potassium bisulfate compound salt was slowly added to the reaction system, stirred at room temperature for 10 minutes, and then placed in a water bath at 50°C for reaction; the progress of the reaction was monitored by liquid chromatography, until the ligustilide chromatographic peak area in the reaction solution was reduced by 80% The reaction was terminated at that time; after the reaction, the insoluble matter was removed by suction filtration, the filtrate was concentrated under reduced pressure at 40°C to remove the solvent, and the residue was separated by pressure silica gel column chromatography (φ30 mm×200 mm), and the mobile phase was petroleum ether-ethyl acetate (6:1, v / v), 20ml / portion of fractions were collected; the fract...
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