2-n-propyl-6-ferrocenyl-imidazo[2,1-b]-1,3,4-thiadiazole preparation method
A ferrocene-based and acetyl-ferrocene technology, applied in chemical instruments and methods, metallocenes, organic chemistry, etc., can solve the problems of low reaction efficiency and long reaction time, so as to improve reaction efficiency and shorten reaction time Effect
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Embodiment 1
[0029] Synthesis method of 2-n-propyl-6-ferrocenyl-imidazo[2,1-b]-1,3,4-thiadiazole
[0030] chemical reaction formula
[0031]
[0032] Synthetic steps:
[0033] (1), mix solid thiosemicarbazide, n-butyric acid and hydrobromic acid, turn on the oil bath to heat and stir, wherein the mass ratio of solid thiosemicarbazide and n-butyric acid is 1:1.15, the mass fraction of hydrobromic acid 50%; heat up to 105°C and keep warm for 4.7 hours, cool to room temperature after the reaction is complete; adjust the pH to 8-9 with 40% sodium hydroxide solution under stirring in an ice-water bath; solids precipitate out of the reaction solution, and stand in an ice-water bath for 30 minutes Fully analyze; filter under reduced pressure, collect the filter cake and dry to obtain the crude product; recrystallize the crude product with 30% ethanol aqueous solution, and dry to obtain 2-amino-5-n-propyl-1,3,4-thiadiazole;
[0034] (2) Stir and mix 2-amino-5-n-propyl-1,3,4-thiadiazole, α-bro...
Embodiment 2
[0042] Synthesis steps of 2-n-propyl-6-ferrocenyl-imidazo[2,1-b]-1,3,4-thiadiazole:
[0043] (1), mix solid thiosemicarbazide, n-butyric acid and hydrobromic acid, turn on the oil bath to heat and stir, wherein the mass ratio of solid thiosemicarbazide and n-butyric acid is 1:1.25, the mass fraction of hydrobromic acid 50%; heat up to 104°C and keep warm for 4.6 hours, cool to room temperature after the reaction is complete; adjust the pH to 8-9 with 39% sodium hydroxide solution under stirring in an ice-water bath; solids precipitate out of the reaction solution, and stand in an ice-water bath for 30 minutes Fully analyze; filter under reduced pressure, collect the filter cake and dry to obtain the crude product; recrystallize the crude product with 30% ethanol aqueous solution, and dry to obtain 2-amino-5-n-propyl-1,3,4-thiadiazole;
[0044] (2) Stir and mix 2-amino-5-n-propyl-1,3,4-thiadiazole, α-bromo-acetylferrocene and ethanol, wherein 2-amino-5-n-propyl- The molar rati...
Embodiment 3
[0052] Synthesis steps of 2-n-propyl-6-ferrocenyl-imidazo[2,1-b]-1,3,4-thiadiazole:
[0053] (1), mix solid thiosemicarbazide, n-butyric acid and hydrobromic acid, turn on the oil bath to heat and stir, wherein the mass ratio of solid thiosemicarbazide and n-butyric acid is 1:1.2, and the mass fraction of hydrobromic acid 50%; heat up to 105°C and keep warm for 4.5 hours, cool to room temperature after the reaction is complete; adjust the pH to 8-9 with 40% sodium hydroxide solution under stirring in an ice-water bath; solids precipitate out of the reaction solution, and stand in an ice-water bath for 28 minutes Fully analyze; filter under reduced pressure, collect the filter cake and dry to obtain the crude product; recrystallize the crude product with 28% ethanol aqueous solution, and dry to obtain 2-amino-5-n-propyl-1,3,4-thiadiazole;
[0054] (2) Stir and mix 2-amino-5-n-propyl-1,3,4-thiadiazole, α-bromo-acetylferrocene and ethanol, wherein 2-amino-5-n-propyl- The molar r...
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