Preparation for paclitaxel, baccatin III and derivates thereof
A derivative, the technology of paclitaxel, applied in the field of paclitaxel, can solve the problems that have not been involved
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Embodiment 1
[0053] Example 1 Preparation of baccatin III by catalyzing acetylation of 10-deacetyl-baccatin III with nitrates of various IIIB metal elements
[0054] Weigh 10-deacetyl-baccatin III (content 98%, see figure 1 ) sample 100mg was dissolved in 1ml reaction solvent, and the nitrate of metal elements of group IIIB of catalytic equivalent was added. 3 The solution quenched the reaction. After the reaction, the feed liquid was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and vacuum rotary evaporated to obtain baccatin III (LC-MS spectrum see figure 2 ). Various catalysts adopted, catalyst amount, reaction solvent, reaction time and yield are shown in Table 1.
[0055] Table 1 Nitrate-catalyzed acetylation of 10-deacetyl-baccatin III by various IIIB metal elements
[0056]
Embodiment 2
[0057] Example 2 Preparation of paclitaxel by catalyzing the acetylation of 10-deacetyl-paclitaxel with nitrates of various IIIB metal elements
[0058] Weigh 10-deacetyl-paclitaxel (content 62%, LC-MS spectrogram see image 3 ) sample 100mg was dissolved in 1ml reaction solvent, and the nitrate of catalytic equivalent IIIB group metal element was added, and after fully mixing, about 5 equivalents of acetic anhydride was slowly added dropwise, stirred at room temperature, and after TLC detected that the reaction was complete, saturated NaHCO was added 3 The solution quenched the reaction. After the reaction, the feed solution was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and vacuum rotary evaporated to obtain 2'-O-acetyl-paclitaxel (LC-MS spectrum see Figure 4 ). Various catalysts adopted, catalyst amount, reaction solvent, reaction time and yield are shown in Table 2.
[0059] Weigh 2'-O-acetyl-paclitaxel (content 55%, LC-MS spectrogram see Figu...
Embodiment 3
[0063] Example 3 Preparation of cephalomannine by 10-deacetyl-cephalomannine
[0064] Weigh 10-deacetyl-cephalomannine (content 85%, LC-MS spectrogram see Figure 6 ) sample 1g, dissolved in 5ml tetrahydrofuran, added 0.1g lanthanum nitrate and mixed thoroughly, slowly added dropwise 0.5ml acetic anhydride, reacted at room temperature for 3 hours, added 25ml saturated NaHCO3 solution to extinguish the reaction. After the reaction, the feed solution was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and vacuum rotary evaporated to obtain 1.03 g of white solid. Dissolve it in 5ml THF, add 2.5ml hydrogen peroxide (concentration 30%), add 100mg sodium citrate, fully dissolve at room temperature, after TLC detects that the reaction is complete, add saturated sodium thiosulfate solution to extinguish the reaction. The feed liquid was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and 0.98 g of white solid was obtained by rotary evaporation un...
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