1,3,4-thiadiazole-containing novel kojic acid derivative and application thereof
A technology of kojic acid derivatives and thiadiazoles, which can be used in pharmaceutical combinations, cosmetic preparations, cosmetics, etc., can solve the problems of easy oxidation and instability of kojic acid, and achieve the effects of easy availability of materials and simple synthesis methods.
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Embodiment 1
[0020] (E)-N-(5-((5-Hydroxy-4-oxo-4H-pyran-2-yl)methylthio)-1,3,4-thiadiazol-2-yl)-3 - Synthesis of (p-tolyl)acrylamide (Ia).
[0021] First place the reaction bottle containing kojic acid (21.0 mmol) in an ice bath, then slowly add 40ml of thionyl chloride dropwise into the reaction bottle and stir it magnetically, and track the reaction progress by TLC. After the reaction is over, add petroleum ether to the reaction solution, a large amount of solids are precipitated, filter, dry the solids and recrystallize with ethanol to obtain the intermediate product 2-chloromethyl-5-hydroxy-4H-pyran-4-one 1 .
[0022] Weigh the above intermediate 1 2-chloromethyl-5-hydroxy-4H-pyran-4-one (10mmol) and 2-amino-5-mercapto-1,3,4-thiadiazole (10mmol) and dissolve in 30ml In ethanol, triethylamine (12mmol) was added dropwise, heated to reflux, and the reaction progress was tracked by TCL. After the reaction was completed, it was cooled to room temperature, and a solid was precipitated. Th...
Embodiment 2
[0027] (E)-N-(5-((5-Hydroxy-4-oxo-4H-pyran-2-yl)methylthio)-1,3,4-thiadiazol-2-yl)-3 -Synthesis of (4-methoxyphenyl)acrylamide (Ib).
[0028] The preparation method of this example is the same as in Example 1 except that p-methoxyphenylacrylic acid is used instead of p-tolylacrylic acid, and finally a white solid (E)-N-(5-((5-hydroxyl-4-oxo -4H-pyran-2-yl)methylthio)-1,3,4-thiadiazol-2-yl)-3-(4-methoxyphenyl)acrylamide, its chemical structural formula is as formula (Ib ), yield: 77.1%.
[0029]
[0030] 1 HNMR (500 MHz, DMSO) δ : 8.59 (s, 1H), 7.81 (s, 1H), 7.77 (d, J = 8.5Hz, 2H), 7.44 (s, 2H), 7.02 (d, J = 8.5 Hz, 2H), 6.70 (d, J = 15.5Hz, 1H),6.47(s, 1H), 4.28(s, 2H), 3.34(s, 3H); 13 CNMR (125 MHz, DMSO) δ IR (KBr) v : 3349, 3110, 1733, 1653,1504, 1418, 1328, 1255, 1201, 1128, 1030 cm -1 ; HRMS (ESI, m / z) calcd for [C 18 h 16 N 3 o 5 S 2 ] + (M+H) + 418.0526, found 418.0527.
Embodiment 3
[0032] (E)-N-(5-((5-Hydroxy-4-oxo-4H-pyran-2-yl)methylthio)-1,3,4-thiadiazol-2-yl)-3 -Synthesis of (3-fluorophenyl)acrylamide (Ic).
[0033] The preparation method of this example is the same as in Example 1 except that 3-fluorophenylacrylic acid is used instead of p-tolylacrylic acid, and finally a white solid (E)-N-(5-((5-hydroxyl-4-oxo -4H-pyran-2-yl)methylthio)-1,3,4-thiadiazol-2-yl)-3-(3-fluorophenyl)acrylamide, its chemical structure is as formula (Ic) As shown, the yield: 74.8%.
[0034]
[0035] 1 HNMR (500 MHz, DMSO) δ : 8.63 (s, 1H), 7.85 (d, J = 16.0 Hz, 1H), 7.75(d, J = 10.0 Hz, 1H), 7.65 (d, J = 8.0 Hz, 1H), 7.50 (q, J = 8.0 Hz, 1H), 7.45 (s, 2H), 7.31 (td, J = 8.5, 2.0 Hz, 1H), 6.96 (d, J = 16.5 Hz, 1H), 6.48(s, 1H), 4.29 (s, 2H); 13 CNMR (125 MHz, DMSO ) δ :171.99, 171.28, 165.09,163.86, 163.58, 161.92, 150.12, 147.68, 146.47, 140.81, 136.68, 136.61,131.48, 131.41, 125.77, 118.34 , 118.17, 118.06, 115.74, 115.42, 115.24,35.94; IR (KBr) v...
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