2-(4-methyl-1,2,3-thiadiazole)-5-(substituent)-1,3,4-oxa(thia)diazole derivative and application thereof
A technology of azole derivatives and thiadiazoles, applied in the field of 2--5--1,3,4-oxadiazole derivatives, which can solve problems such as uneven color, reduced quality, and poor smoke taste
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[0044] Example :Synthesis of target compound
[0045] Synthesis of 2-(4-methyl-1,2,3-thiadiazole)-5-(substituent)-1,3,4-oxadiazole derivatives
[0046] Synthesis of intermediate ethyl carbazate
[0047]
[0048] Put diethyl carbonate (11.8g, 0.1mol) and 80% hydrazine hydrate (5.9g, 0.095 mol) into a 100 mL three-necked flask, stir at room temperature (23℃) for 4h, TCL followed the reaction (iodine color, V petroleum Ether: V ethyl acetate=3:1). The ethanol and water were removed under reduced pressure, and colorless crystals were precipitated. The product was obtained with a pumping rate of 9g, with a melting point of 44~45℃ (45~46℃, Fan, Z. J., et al, 2009), and a yield of 87%.
[0049] Synthesis of condensation intermediates
[0050]
[0051] Put ethyl acetoacetate (6.5g, 0.05 mol) and dichloromethane (35 mL) into a 100 mL three-necked flask, and dissolve ethyl carbazate (5.2g, 0.05 mol) in dichloromethane (17 mL) Then slowly drip into the three-necked bottle, the dripping is comp...
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