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CAS No. : | 6268-43-5 | MDL No. : | MFCD00233705 |
Formula : | C11H10N4O | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | FOQXHWCMYZXOGZ-UHFFFAOYSA-N |
M.W : | 214.22 | Pubchem ID : | 80445 |
Synonyms : |
|
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | |
GHS Pictogram: |
* 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 |
---|---|---|
62% | With iron(II,III) oxide; ferric hydroxide; In para-xylene; at 140℃; for 60.0h; | 1 ,3-di(Pyridin-2-yl)urea (5a) was synthesised via the reaction of triphosgene (1 .0 g, 3.37 mmol) with 2-aminopyridine (6a) (1.576 g, 16.74 mmol) in the presence of DMAP (2.44 g, 20.01 mmol) in 0H2012(15.0 mL) at room temperature for 36 h. 5a was equally synthesised via Fe(OH)3Fe304-catalysed(0.060 g, 0.052 mmol) reaction of 2-aminopyridine (6a) (0.376 g, 4.0 mmol) with urea (3b) (0.120 g,2.0 mmol) in p-xylene at 140 00 for 2.5 days and obtained in 62% (0.266 g, 1.24 mmol) yield.26 White crystals; m.p. 175 c 130-NMR (100 MHz, DMSO-d6): : 152.4, 151.9, 147.3, 138.4, 118.1, 112.4. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With diethylene glycol dimethyl ether; cesium fluoride; at 100℃; for 20.0h;Schlenk technique; Glovebox; | General procedure: In the glove box, add aniline (1mmol), CsF (2mol), and diglyme (3mL) to the 10ml Schlenk bottle, and replace the air with CO2. Connect the Schlenk bottle with a CO2 balloon, and then PMHS with a syringe (4.5 mmol) was poured into a reaction flask and placed in an oil bath and stirred at 100 C for 20 hours. After the reaction was completed, the temperature was lowered to room temperature, and then poured into 30 mL of H2O, and a large amount of precipitate was immediately obtained, and then a large amount of solid powder was obtained by suction filtration. The solid powder was washed with n-hexane (3 x 5 mL) to remove unreacted raw materials, and then ethyl acetate was used. (3 x 10 mL) washed the solid powder. The ethyl acetate layer was collected, dried over anhydrous magnesium sulfate, and then subjected to vacuum rotary evaporation to obtain a pure product in an isolated yield of 96%. |
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