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CAS No. : | 1175275-00-9 | MDL No. : | MFCD16659787 |
Formula : | C15H25BN2O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | WCTWBVYTYXBCRR-UHFFFAOYSA-N |
M.W : | 276.18 | Pubchem ID : | 57345810 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-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 |
---|---|---|
41% | With tetrakis(triphenylphosphine) palladium(0); caesium carbonate; In 1,4-dioxane; water; at 100.0℃;Inert atmosphere; Sealed tube; | EXAMPLE 8 SYNTHESIS OF 5-(l-CYCL0HEXYL-lH-PYRAZ0L-4-YL)-3-(5-PHENYL-l,2,4-0XADiAZ0L-3- In a sealed tube, a mixture of 5-bromo-3-(5-phenyl-l,2,4-oxadiazol-3- yl)pyridin-2-amine (70.0 mg, 0.221 mmol), l-cyclohexyl-4-(4,4,5,5-tetramethyl-l,3,2- dioxaborolan-2-yl)-lH-pyrazole (61.0 mg, 0.221 mmol) and cesium carbonate (145 mg, 0.442 mmol) in 1 ,4-dioxane/water (2.0 mL, 4:1) was degassed with nitrogen gas for 10 minutes, followed by the addition of tetrakis(triphenylphosphine)palladium (26.0 mg, 22.1 muetaiotaomicron). The mixture was degassed for another 10 minutes. The resulting mixture was sealed and heated at 100 C overnight. After cooled to ambient temperature, the reaction mixture was filtered through a celite cake, and washed with dichloromethane and methanol. The filtrate was concentrated and the residue was treated with dichloromethane/methanol, and filtered. The filtrate was concentrated and the residue was purified by column chromatography eluted with dichloromethane :methanol from 100:1 to 50:1 to afford the title compound as a white solid in 41% yield (35 mg). 1H NMR (400 MHz, CDC13): delta 8.52 (d, J= 2.4 Hz, 1H), 8.40 (d, J= 2.4 Hz, 1H), 8.28- 8.23 (m, 2H), 7.79 (s, 1H), 7.70 (s, 1H), 7.68-7.63 (m, 1H), 7.62-7.56 (m, 2H), 6.25- 6.10 (br s, 2H), 4.21-4.12 (m, 1H), 2.27-2.20 (m, 2H), 2.00-1.90 (m, 2H), 1.85-1.74 (m, 3H), 1.54-1.40 (m, 2H), 1.37-1.25 (m, 1H). MS (ES+): m/z 387.3 (M + 1), 409.4 (M + Na). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
20% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In dimethyl sulfoxide; at 90.0℃; for 20.0h; | 3. To a solution of 4-bromo-l -cyclohexyl- lH-pyrazole (1.13 g, 4.95 mmol) in dimethyl sulfoxide (10 mL) was added potassium acetate (1.47 g, 15 mmol), pinacol diboron (1.52 g, 6.00 mmol). The mixture was degassed for 10 min, followed by the addition of PdCl2(dppf) (0.300 g, 0.400 mmol). The mixture was degassed for another 10 min and heated at 90 C for 20 h, diluted with ethyl acetate (80 mL), washed with water (2 x 20 mL), brine (20 mL) and dried. The residue after removal of the solvents was purified by flash column chromatography eluted with 10% ethyl acetate in hexanes to afford l-cyclohexyl-4-(4,4,5,5-tetramethyl-l,3,2-dioxaborolan-2-yl)-lH- pyrazole as a white solid in 20% yield (0.265 g). 1H NMR (300 MHz, CDC13) delta 7.80 (s, 1H), 7.75 (s, 1H), 4.21-4.11 (m, 1H), 2.21-2.14 (m, 2H), 1.94-1.85 (m, 2H), 1.77-1.65 (m, 3H), 1.48-1.34 (m, 3H), 1.32 (s, 12H). |
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