A kind of octahydroacridine skeleton with three continuous chiral centers and preparation method thereof
A technology of octahydroacridine and skeleton, which is applied in the field of octahydroacridine skeleton and its preparation, and can solve the problems of low universality of the skeleton, low yield of octahydroacridine, complex synthesis process, etc.
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Embodiment 1
[0040]Dissolve 0.2 mmol of N-Ts anthranilaldehyde in 1 mL of a mixed solvent of pyridine and toluene (the volume ratio of pyridine to toluene is 7:3), then add 0.04 mmol of catalyst silane-modified 4-hydroxyproline, and then add 0.5 mmol cyclohexenone, then immediately placed in a constant temperature ice bath, and kept the reaction temperature at 0 ° C, after 10 hours of reaction, spot the plate, after confirming the completion of the reaction, pass the reaction solution through the chromatographic column, and use a volume ratio of 25% Ethyl acetate and petroleum ether were used for elution to obtain 69.8 mg of a white solid with a yield of 94%. The solid was tested by optical rotation, infrared, nuclear magnetic, high performance liquid chromatography and mass spectrometry.
[0041] Infrared test results such as figure 1 As shown in (a), from figure 1 (a) It can be seen that it is at 3475, 2948, 2872, 2171, 1695, 1618, 1479, 1456, 1415, 1350, 1244, 1166, 1122, 1068, 935, 86...
Embodiment 2
[0050] Dissolve 0.2mmol of 5-fluoro-N-Ts anthranilaldehyde in 1mL of a mixed solvent of pyridine and toluene (the volume ratio of pyridine to toluene is 7:3), and then add 0.04mmol of catalyst silane-modified 4-hydroxyproline , and then add 0.5mmol cyclohexenone, then immediately put it in a constant temperature ice bath, and keep the reaction temperature at 0°C, after 10 hours of reaction, spot the plate, after confirming that the reaction is complete, pass the reaction solution through the chromatographic column, and use Eluting with ethyl acetate and petroleum ether at a volume ratio of 25%, 69.8 mg of a white solid was obtained with a yield of 94%. The solid was tested by optical rotation, infrared, NMR, high performance liquid chromatography and mass spectrometry.
[0051] Infrared test results such as figure 1 As shown in (b), the product of this embodiment is at 3416,2948,2171,1693,1479,1426,1350,1248,1165,1137,942,911,880,818,679,612,544cm -1 There are characteristic ...
Embodiment 3
[0060] Dissolve 0.2mmol of 5-chloro-N-Ts anthranilaldehyde in 1mL of a mixed solvent of pyridine and toluene (the volume ratio of pyridine to toluene is 7:3), then add 0.04mmol of 4-hydroxyproline modified by catalyst silane , and then add 0.5mmol cyclohexenone, then immediately put it in a constant temperature ice bath, and keep the reaction temperature at 0°C, after 10 hours of reaction, spot the plate, after confirming that the reaction is complete, pass the reaction solution through the chromatographic column, and use Eluting with ethyl acetate and petroleum ether at a volume ratio of 15%, 77.8 mg of a white solid was obtained with a yield of 96%. The solid was tested by optical rotation, infrared, NMR, high performance liquid chromatography and mass spectrometry.
[0061] Infrared test results such as figure 1 As shown in (c), the product of this example is at 3929,3415,3237,2944, 2171,1692,1638,1618,1470,1417,1349,1305,1249,1164,1128,1088,1033,934, 820,709,670,622cm -1 ...
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