New usage of zedoary cyclic diolefine
A technology for cyclodiene and medicament of turmeric, applied in the field of cyclodiene derivatives of turmeric, can solve the problems of yellowing, cyclodiene of turmeric is unstable, easy to decompose, etc., achieves short operation period, avoids decomposition and transformation , the effect of high degree of separation
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preparation example 1
[0023] Preparation Example 1: Preparation of Potentiocycladiene
[0024] Take 1.5 kg of curcuma medicinal material, grind it into coarse powder (pass through No. 2 sieve), put it into the HA221-50-06 supercritical extraction device, under the pressure of 28Mpa, 60 ℃, CO 2 The flow rate was 25kg / hr and extraction was carried out for 1.5 hours. The pressures of the analysis kettles I and II were 10 and 6Mpa respectively, and the temperatures were 50 and 45°C respectively. 120g of yellow or brown oily extract was obtained by analysis, and the extraction yield was 8.0%. Place the extract in the refrigerator, precipitate crystals and wash with methanol to obtain white needle-like crystals, mp.69-71°C. Identified by UV, IR, NMR, MS and other spectral techniques, the molecular formula C 15 h 20 O, with a molecular weight of 216.32, has a structure of zedoary cyclodiene.
[0025] IR(KBr): 3052, 3027(=CH), 2968, 2928, 2890, 2856, 1622(C=C), 1552(C=C, Furan), 1445, 1385(CH 3 , CH 2...
preparation example 2
[0032] Preparation example 2: preparation of the reference substance of zedoary cyclodiene
[0033] Take 1.5 kg of curcuma medicinal material, grind it into coarse powder (pass through No. 2 sieve), put it into the HA221-50-06 supercritical extraction device, under the pressure of 28Mpa, 60 ℃, CO 2 The flow rate is 25kg / hr and extraction is carried out for 1.5 hours. The pressures of the analysis kettles I and II are respectively 10 and 6Mpa, and the temperatures are respectively 50 and 45°C. After analysis, 120g of yellow or brown oily extract is obtained. Take 60g of 100-200 mesh silica gel, Pack the column by dry method, load 2g of oily extract, elute with 300ml petroleum ether, after the eluent is drained, the silica gel is divided into two distinct colored bands, cut off the red silica gel, add 100ml of ethyl acetate, sonicate for 30min, and filter , repeated 3 times, combined the filtrates, recovered ethyl acetate, added methanol to slightly heat the residue to dissolve ...
preparation example 3
[0034] Preparation Example 3: Preparation of 2-Acetyl-Pengcuracyclodiene
[0035]Add 0.10 mol of zedoary cyclodiene compound, 0.15 mol of aluminum trichloride, and 40 ml of carbon disulfide into a three-necked flask equipped with a reflux condenser and a dropping funnel. Dilute 0.10 mol of acetyl chloride with an appropriate amount of carbon disulfide in the dropping funnel, and slowly add it into the three-necked bottle under mechanical stirring (about 1-2 drops / second). After the addition, stir at room temperature for 2 hours, and react for 2 hours. After the reaction is completed, slowly add about 20ml of concentrated hydrochloric acid diluted with 1:1 (v / v) water to the three-necked flask under ice bath, The solution was layered, and when the solid in the three-necked flask was fully dissolved, it was cooled, transferred to a 500ml separatory funnel and extracted several times with chloroform, discarded the water layer, combined the chloroform layers, added 50ml of 10% NaO...
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