A kind of synthetic method of 1,3,4-thiadiazole derivatives
A technology of thiadiazole derivatives and synthetic methods, which is applied in organic chemistry and other fields, and can solve problems such as high manufacturing cost, low reaction yield, and large environmental hazards
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Embodiment 1
[0025] (1) Synthesis of Compound Ⅰ(a): Into a 500 mL four-necked flask were sequentially added 50.6 g (0.50 mol) of trimethylacetic acid, 46.8 g (0.75 mol) of 80% hydrazine hydrate, and active Al 2 O 3 5g, 100mL of toluene, turn on stirring, heat up and reflux for dehydration, dehydrate to anhydrous, cool down and filter to remove active Al 2 O 3 , and the obtained trimethyl acetohydrazide toluene solution is to be cast in the next step.
[0026] (2) Synthesis of compound II (a): add toluene 150mL, KSCN 53.5g (0.55mol) to a 500mL four-necked flask, turn on stirring, slowly heat up, and slowly add methyl chloroformate 47.3g ( 0.50mol), after the dropwise addition, continue to keep stirring for 1h, cool down to room temperature, and the obtained methyl isothiocyanate toluene solution is to be put into the next step.
[0027] (3) Synthesis of compound III (a): at room temperature, the toluene solution of the above-mentioned trimethyl acetohydrazide was slowly added dropwise t...
Embodiment 2
[0032] (1) Synthesis of Compound Ⅰ(b): Into a 500 mL four-necked flask were sequentially added 44.1 g (0.50 mol) of isobutyric acid, 46.8 g (0.75 mol) of 80% hydrazine hydrate, and active Al 2 O 3 5g, 100mL of xylene, turn on stirring, heat up and reflux for dehydration, to anhydrous, remove the active Al by cooling and filtration 2 O 3 , the obtained isobutyryl hydrazide xylene solution is for the next step.
[0033] (2) Synthesis of compound II (b): add 150 mL of xylene and 44.6 g (0.55 mol) of NaSCN to a 500 mL four-necked flask, turn on stirring, slowly heat up, and slowly add 54.2 g of ethyl chloroformate dropwise at 55°C (0.50mol), after the dropwise addition was completed, continue to keep stirring for 1 hour, cool down to room temperature, and the obtained xylene solution of ethyl isothiocyanate formate is to be put into the next step.
[0034] (3) Synthesis of compound III (b): at room temperature, the xylene solution of the above isobutyryl hydrazide was slowly a...
Embodiment 3
[0039] (1) Synthesis of compound I(c): Into a 500 mL four-necked flask were sequentially added 57.1 g (0.50 mol) of trifluoroacetic acid, 46.8 g (0.75 mol) of 80% hydrazine hydrate, 1 g of isopropyl titanate, and 100 mL of xylene , turn on stirring, heat up and reflux for dehydration until anhydrous is removed, cool down to room temperature, and the obtained trifluoroacetazide xylene solution is to be put into the next step.
[0040] (2) Synthesis of compound II (c): add 150 mL of xylene and 44.6 g (0.55 mol) of NaSCN to a 500 mL four-necked flask, turn on stirring, slowly heat up, and slowly add benzyl chloroformate 85.3 g dropwise at 65°C (0.50mol), after the dropwise addition was completed, continue to keep stirring for 1 h, cool down to room temperature, and obtain the benzyl isothiocyanate xylene solution for the next step.
[0041] (3) Synthesis of compound III (c): at room temperature, the xylene solution of the above trifluoroacetazide was slowly added dropwise to the ...
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