Method for preparing oteconazole intermediate
A technology of oteconazole and intermediates, applied in the field of medicinal chemistry, can solve the problems of unfavorable industrialization and high price of Pt, and achieve the effect of complete reaction, less impurities, and easy industrial application
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reference example 1
[0034]
[0035] Referring to the preparation method of Example 4 of CN108289457B, the reduction reaction is carried out with Pt as a catalyst. After the reduction reaction is completed, the reaction solution is sampled and detected. figure 1 , the area percentage report is shown in Table 1.
[0036] Table 1 Area Percentage Report
[0037]
reference example 2
[0038] Reference Example 2: Using Raney nickel as catalyst and methanol as solvent
[0039] Add 20g of formula II intermediate, add 100g (5w / w) ethanol, add 2g (0.1w / w) Raney nickel, replace with nitrogen, replace with hydrogen, pressurize to 0.1MPa, keep the reaction at 20~25℃ for 10 hours, The reaction was confirmed to be complete by HPLC. Sampling and testing the reaction solution, see the spectrum of related substances figure 2 , the area percentage report is shown in Table 2. Refer to Example 4 of CN108289457B for post-treatment to obtain 14.6 g of the semi-L-DTTA salt of the compound of formula I, with a yield of 52%.
[0040] Table 2 Area Percentage Report
[0041]
Embodiment 1
[0042] Embodiment 1: take Raney nickel+acetic acid as catalyst, methanol is solvent
[0043] Add 20g of formula II intermediate, add 200g (10w / w) methanol, add 1.8g (0.6eq) acetic acid, add 4g (0.2w / w) Raney nickel, nitrogen replacement, hydrogen replacement, pressurize to 0.3MPa, at The reaction was incubated at 20-30°C for 8 hours, and the completion of the reaction was confirmed by HPLC. Sampling and testing the reaction solution, see the spectrum of related substances image 3 , the area percentage report is shown in Table 3. After the reaction solution was filtered, the solution was decompressed to dryness, and 60 g of isopropanol was added to continue the precipitation, and then 160 g of isopropanol was added, and the temperature was increased to dissolve. The mixture was kept at 20-30° C. for 16 hours, filtered and dried to obtain 21.3 g of the semi-L-DTTA salt of the compound of formula I, with a yield of 76%.
[0044] Table 3 Area Percentage Report
[0045]
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