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CAS No. : | 6336-32-9 | MDL No. : | MFCD09879258 |
Formula : | C18H12N2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | YCPBCVTUBBBNJJ-UHFFFAOYSA-N |
M.W : | 256.30 | Pubchem ID : | 95838 |
Synonyms : |
|
Signal Word: | Warning | Class: | |
Precautionary Statements: | P280 | UN#: | |
Hazard Statements: | H302-H317 | 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 |
---|---|---|
35% | With copper; potassium carbonate; at 180℃; for 31h;Inert atmosphere; | A nitrogen gas atmosphere was prepared in a reaction vessel equipped with a stirrer, then, a compound 13 (0.8 g) synthesized according to a method described in ?JP-A No. 2011-216484?, 4-n-butyliodobenzene (2.3 g), copper (1.5 g), potassium carbonate (1.6 g) and tetraethylene glycol dimethyl ether (19 ml) were added, and the mixture was stirred at 180 C. for 31 hours. The resultant reaction liquid was cooled down to room temperature, then, water and toluene were added, and the mixture was stirred at room temperature. The resultant organic layer was analyzed HPLC (high performance liquid chromatography) to resultantly observe generation of a compound 15 as the target compound at a yield of 85%. Thereafier, the aqueous layer was separated, and the organic layer was washed with a saturated sodium chloride aqueous solution. To the resultant organic layer was added magnesium sulfate, then, the layer was filtrated, and concentrated to obtain a coarse product.The resultant coarse product was washed with heptane several times, then, recrystallized using toluene, thereby obtaining 0.6 g of a compound 15 (yield: 35%, purity:95.8%) as a white solid. ?H-NMR (THF-d5, 300 MHz): oe (ppm)=1.08 (6H, m), 1.57 (4H, m), 1.85 (4H, m), 2.85 (4H, t), 7.21 (2H, m), 7.40 (4H, m), 7.58 (4H, d), 7.67 (4H, d), 8.19 (4H, m). |
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