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CAS No. : | 872365-91-8 | MDL No. : | MFCD16140194 |
Formula : | C6H4BrF2N | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | ZTBGDNNRDRISQZ-UHFFFAOYSA-N |
M.W : | 208.00 | Pubchem ID : | 10104489 |
Synonyms : |
|
Signal Word: | Danger | Class: | 6.1 |
Precautionary Statements: | P301+P310+P330-P302+P352-P305+P351+P338 | UN#: | 2810 |
Hazard Statements: | H301-H315-H319 | Packing Group: | Ⅲ |
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 |
---|---|---|
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In 1,4-dioxane; at 110℃; for 20h;Inert atmosphere; | To the reaction mixture of 2-bromo-6-(difluoromethyl)pyridine (1.55 g, 7.45 mmol), ethyl 2-(4-(4,4 ,5 ,5 -tetramethyl- 1,3 ,2-dioxaborolan-2-yl)cyclohex-3 -en-iyl)acetate (2.52 g, 8.57 mmol) in 1,4-Dioxane (20 mL) was added K2C03 (7.45 mL, 22.36 mmol) solution and the resulting mixture was purged with nitrogen stream for 3mm, followed by addition of Pd(Ph3P)4 (0.43 1 g, 0.373 mmol) and the reaction mixture was further purged with nitrogen stream and then heated at 110 C under nitrogen for 20 h. The reaction mixture was diluted with brine and ethyl acetate. The organic layer was separated, dried over MgSO4. The filtrate was concentrated in vacuo.and the residue was purified via silica gel flash column chromatography, eluting with 0-20% ethyl acetate inhexane to give Intermediate 231A (oil, 2.2 g, 7.45 mmol, 99% yield). LC-MS Anal.Calc’d for C,6H,9F2N02, 295.14, found [M+H] 296.2 . T = 1.10 mm (Method A). ‘HNMR (400MHz, METHANOL-d4) ö: 7.92 - 7.80 (m, 1H), 7.60 (dd, J=8.0, 0.8 Hz, 1H),7.47 (d, J7.7 Hz, 1H), 6.71 (dd, J3.1, 2.0 Hz, 1H), 6.65 - 6.44 (m, 1H), 4.20 - 4.08 (m,2H), 2.79 - 2.65 (m, 1H), 2.56 - 2.39 (m, 2H), 2.36 (d, J=7.0 Hz, 2H), 2.20 - 1.92 (m, 3H),1.48 (dtd,J=13.0, 10.6, 5.5 Hz, 1H), 1.30- 1.22 (m, 3H) |
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