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CAS No. : | 734533-08-5 | MDL No. : | N/A |
Formula : | C10H11N3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 173.21 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P330-P363-P501 | UN#: | N/A |
Hazard Statements: | H302-H312-H332 | Packing Group: | N/A |
GHS Pictogram: |
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* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | In diethyl ether soln. of org. compd. added to stirred soln. of Sn compd. at room temp., stirred for 6 h at room temp.; filtered, washed with ether, dried in vac.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | In diethyl ether soln. of org. compd. added to stirred soln. of Sn compd. at room temp., stirred for 6 h at room temp.; filtered, washed with ether, dried in vac.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | In diethyl ether soln. of org. compd. added to stirred soln. of Sn compd. at room temp., stirred for 6 h at room temp.; filtered, washed with ether, dried in vac.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; ammonia aq. NH3; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ammonia; acetonitrile aq. NH3; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium dichromate; sulfuric acid; water; nitric acid Reflux; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With nitric acid at 140℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrazine hydrate In toluene at 20℃; | ||
700 mg | With hydrazine hydrate In toluene at 20℃; for 24h; | |
With hydrazine hydrate In chloroform at 20℃; | 1.1; 2.1; 3.1 (1) Synthesis of ligand 3,5-dimethyl-4-(4'-pyridyl)-pyrazole (HL, C10H11N3) At -20°C, dissolve 36.5mL of 4-picoline (372 mmol) in 50mL of CHCl3, add 21.2mL of acetyl chloride (300 mmol) dropwise within 10-15min with a separatory funnel under stirring conditions , after stirring for 60min, the solution turns dark green, and the reaction is continued for 5h,A brownish-yellow liquid is obtained, and a brown solid is obtained by distillation under reduced pressure. After dissolving the solid solution in toluene, a yellow solution and a brown 4-picoline hydrochloride insoluble in toluene are obtained, and the 4-picoline hydrochloride is removed by suction filtration under reduced pressure. hydrochloride, the resulting filtrate was purified by thin-layer chromatography to obtain a yellow oily substance 3-(pyridin-4-yl)pentane-2,4-dione, which was added to 3-(pyridin-4-yl ) pentane-2,4-dione was added 6mL hydrazine hydrate for ring closure, stirred at room temperature for 17h, and the solvent was distilled off under reduced pressure to obtain a mixture of ligand HL and a small amount of impurities, and water was added to the resulting mixture (the ratio of solid to liquid was 1g : 325mL), recrystallized at -4°C to obtain colorless crystals, after drying (60°C, 5h), a white solid powder was obtained, which was the ligand 3,5-dimethyl-4-(4'-pyridine base)-pyrazole (HL). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water-d2 at 20℃; for 12h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water-d2 at 100℃; for 5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | With tetrabutylammomium bromide; sodium hydroxide In water; benzene for 48h; Reflux; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: chloroform / 4 h / -20 °C / Inert atmosphere 2: hydrazine hydrate / toluene / 24 h / 20 °C | ||
Multi-step reaction with 2 steps 1: acetyl chloride / chloroform 2: hydrazine hydrate / chloroform / 17 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80 % | In methanol at -5 - 140℃; Sealed tube; | 1.2; 2.2; 3.3 (2) Synthesis of cyclic trinuclear cuprous complex (Complex 1) Add 1.5 mg Cu(OH)2 (0.015 mmol), 5.2 mg of the ligand HL (0.03 mmol) obtained in step (1) and 3 mL of methanol into a hard glass tube with an inner diameter of 8 mm, seal the tube with a hydrogen-oxygen flame machine, and naturally After cooling, place it in a constant temperature oven, raise the temperature to 140°C within 10 minutes, keep it for 72 hours, then lower it to room temperature at a rate of 5°C/h, open the tube to filter, wash with absolute ethanol, and dry naturally to obtain colorless needle-shaped crystals , which is Complex 1, and the yield is 80%. |