A kind of preparation method of rapamycin
A technology of rapamycin and ethyl acetate, which is applied in the field of preparation of high-purity rapamycin, can solve the problems of difficult separation and extraction of rapamycin, low rapamycin fermentation yield, and low separation efficiency. Reach the effect of reducing initial equipment investment, low equipment requirements, and high purification efficiency
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Embodiment 1
[0041] 30L fermentation broth (HPLC chromatogram as shown in figure 1 as shown, figure 1 The corresponding retention time and peak area are shown in Table 1) Press filtration to obtain 2.5kg mycelia. 10L of acetone was added to the mycelia, stirred for 4 hours, and filtered to obtain 10.3L of filtrate, which was detected by HPLC to contain 31.5g of rapamycin. Concentrate with a rotary evaporator at 50° C. under a vacuum of -0.09 MPa until no acetone flows out to obtain 1.8 L of a concentrated solution. 7.2 L of ethyl acetate was added to the concentrated solution, stirred for 30 minutes, and the layers were separated in a separatory funnel, and the ethyl acetate layer was collected to obtain a 7.1 L ethyl acetate layer. Add 7.1L 3%NaHCO 3 The solution was stirred and washed, and the water layer was discarded after separation, and the washing was repeated three times. Finally, 7 L of ethyl acetate layer was obtained. Add 140 g of activated carbon to the ethyl acetate layer...
Embodiment 2
[0047] Take 3L of blank silica gel and pack it into a column with petroleum ether, with a diameter-to-height ratio of 1:9. The loaded silica gel obtained in Example 1 was loaded into a silica gel column by dry loading. Pre-wash with 6L petroleum ether: ethyl acetate as 2:8 prewash; then prewash with 6L petroleum ether: ethyl acetate as 3:7 prewash; then use 6L petroleum ether: ethyl acetate as 4 :6 pre-washing solution; finally pre-washing with 6L petroleum ether:ethyl acetate as 5:5 pre-washing solution. After prewashing, desorb with petroleum ether:ethyl acetate ratio of 7:13. Collect higher purity fractions. The desorption mixture was concentrated to a dry powder at 50°C and a vacuum of -0.09MPa. Obtained 29.3 g of off-white crude product I, HPLC purity: 88.5%. (HPLC chromatogram as image 3 , image 3 The corresponding retention time and peak area are shown in Table 3).
[0048] table 3:
[0049] .
Embodiment 3
[0051] The crude product I was dissolved in 1500ml of acetonitrile, and 1500ml of purified water was added with stirring. Adsorbed by 9L UniPS40 macroporous resin, desorbed with 50% acetonitrile after the adsorption was completed, collected components with higher purity, and obtained 27L desorbed mixed solution. The desorption mixture was concentrated at 40°C under a vacuum of -0.095MPa. Cool the concentrated solution to 4°C~8°C, add an equal volume of dichloromethane at a temperature of 4°C~8°C to the concentrated solution, stir for 30 minutes, put it in a separatory funnel to separate layers, and collect the methylene chloride layer. Anhydrous sodium sulfate was added to dichloromethane, stirred and dehydrated at 4°C~8°C for 5 hours, the dichloromethane layer was obtained by suction filtration, and concentrated to dryness under vacuum to obtain 24.9g of crude product II, HPLC purity: 99.6%. (The HPLC chromatogram of crude product II is as Figure 4 , Figure 4 The corresp...
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