Method for synthesizing polypyrazole vesicles in one step
A technology of polypyrazole vesicles and compounds, applied in the field of one-step synthesis of polypyrazole vesicles, which can solve the problems of many influencing factors and many synthesis steps
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Embodiment 1
[0034] (1) Add p-toluenesulfonyl hydrazide (9.32 g, 50.0 mmol) and p-toluenesulfonyl chloride (14.3 g, 75 mmol) into 50 mL of dichloromethane, stir at room temperature to form a suspension, and slowly add pyridine (6.0 mL, 75.0 mmol). After 1.5 h at 0 o Add 200 mL ether and 100 mL deionized water to C and stir for 15 min. The obtained white solid was dissolved in 400 mL of methanol, the methanol was distilled under reduced pressure to remove 200 mL of methanol, recrystallized at low temperature, and the solvent was removed by suction filtration to obtain bis(p-toluenesulfonyl)hydrazine, which was dried in a vacuum Dried in a container.
[0035] (2) Add 3-butyn-1-ol (1.4 g, 20 mmol) and sodium bicarbonate (5.04 g, 60.0 mmol) into 1000 mL of acetonitrile and dissolve at 0 o Bromoacetyl bromide (6.05 g, 30 mmol) was slowly added dropwise at C. After 10 min, the reaction was quenched with 100 mL of deionized water and extracted with dichloromethane and saturated sodium chlorid...
Embodiment 2
[0038] (1) Add p-toluenesulfonyl hydrazide (9.32 g, 50.0 mmol) and p-toluenesulfonyl chloride (14.3 g, 75 mmol) into 50 mL of dichloromethane, stir at room temperature to form a suspension, and slowly add pyridine (6.0 mL, 75.0 mmol). After 1.5 h at 0 o Add 200 mL ether and 100 mL deionized water to C and stir for 15 min. The obtained white solid was dissolved in 400 mL of methanol, the methanol was distilled under reduced pressure to remove 200 mL of methanol, recrystallized at low temperature, and the solvent was removed by suction filtration to obtain bis(p-toluenesulfonyl)hydrazine, which was dried in a vacuum Dried in a container.
[0039] (2) Add propynyl alcohol (1.12 g, 20 mmol) and sodium bicarbonate (5.04 g, 60.0 mmol) into 1000 mL of acetonitrile and dissolve at 0 o Bromoacetyl bromide (6.05 g, 30 mmol) was slowly added dropwise at C. After 10 min, the reaction was quenched with 100 mL of deionized water and extracted with dichloromethane and saturated sodium ch...
Embodiment 3
[0041] (1) Add p-toluenesulfonyl hydrazide (9.32 g, 50.0 mmol) and p-toluenesulfonyl chloride (14.3 g, 75 mmol) into 50 mL of dichloromethane, stir at room temperature to form a suspension, and slowly add pyridine (6.0 mL, 75.0 mmol). After 1.5 h at 0 o Add 200 mL ether and 100 mL deionized water to C and stir for 15 min. The obtained white solid was dissolved in 400 mL of methanol, the methanol was distilled under reduced pressure to remove 200 mL of methanol, recrystallized at low temperature, and the solvent was removed by suction filtration to obtain bis(p-toluenesulfonyl)hydrazine, which was dried in a vacuum Dried in a container.
[0042] (2) Add 1-phenyl-2-propyn-1-ol (3.64 g, 20 mmol) and sodium bicarbonate (5.04 g, 60.0 mmol) into 1000 mL of acetonitrile and dissolve at 0 o Bromoacetyl bromide (6.05 g, 30 mmol) was slowly added dropwise at C. After 10 min, the reaction was quenched with 100 mL of deionized water and extracted with dichloromethane and saturated sod...
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