Inhibitor of glyceraldehyde-3-phosphate dehydrogenase, preparation method and application thereof
A technology of glyceraldehyde phosphate dehydrogenase and inhibitors, applied in the field of inhibitors of glyceraldehyde phosphate dehydrogenase and its preparation, can solve the problems of twice the result with half the effort in cancer drug treatment, and achieve good anticancer activity
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Embodiment 1
[0022] Embodiment 1 compound 1, the synthesis of 3-bromo-2 oxopropionic acid phenylethyl ester
[0023]
[0024] Add concentrated sulfuric acid (87μL, 1.64mmol) to the turbid solution of magnesium sulfate (788mg, 6.55mmol) in anhydrous dichloromethane (4mL), stir at room temperature for half an hour, then add 3-bromopyruvate (410mg, 2.46mmol) and phenylethyl alcohol (0.2 mL, 1.64 mmol). The reaction was carried out at room temperature, and the progress of the reaction was monitored by TLC and 1H-NMR. After the reaction, the reaction solution was diluted with dichloromethane, filtered under reduced pressure with a funnel covered with diatomaceous earth, and the filtrate was washed with saturated brine to remove excess 3-bromopyruvate, then dried with anhydrous sodium sulfate, and finally The solvent was evaporated under reduced pressure and dried in vacuo to obtain 1 as an orange liquid with a yield of 95%. 1 HNMR (400MHz, CDCl 3 ): δ7.36-7.26(m, 5H), 4.55(t, J=7.2Hz, 2H)...
Embodiment 2
[0025] Embodiment 2, compound 2, the synthesis of 3-bromo-2 oxopropionic acid-1-phenylethyl-ester
[0026]
[0027] Using the same conditions for the synthesis of phenylethyl 3-bromo-2-oxopropionate 1, 2 was successfully prepared as a green liquid with a yield of 93%. 1 HNMR (400MHz, CDCl 3 ):δ7.41-7.32(m,5H),6.03(q,J=6.4Hz,1H),4.30(s,2H),1.68(d,J=6.8Hz,3H); 13 CNMR (100MHz, CDCl 3 ): δ184.6, 158.7, 139.8, 128.7, 128.6, 127.0, 126.3, 76.0, 30.8, 21.9; IR (KBr, cm-1): υ1733, 1390, 1274, 1163, 1053.
Embodiment 3
[0028] Embodiment 3, the synthesis of compound 3,3-bromo-2 oxopropionic acid 3-pentyl ester
[0029]
[0030] Using the same conditions for the synthesis of phenylethyl 3-bromo-2-oxopropionate 1, 3 was successfully prepared as a yellow liquid with a yield of 72%. 1 HNMR (400MHz, CDCl 3 ):δ4.97-4.91(m,1H),4.29(s,2H),1.73-1.66(m,4H),0.954-0.910(m,6H); 13 CNMR (100MHz, CDCl 3 ): δ185.1, 159.5, 80.9, 30.7, 26.3, 9.5; IR (KBr, cm-1): υ1736, 1399, 1265, 671.
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