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Krzysztof Kuciński ; Grzegorz Hreczycho ; ChemCatChem,2022,14(18):e202200794. DOI: 10.1002/cctc.202200794
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Abstract: Commercially available and inexpensive potassium bis(trimethylsilyl)amide (KHMDS) serves as an efficient transition metal-free catalyst for the catalytic sp C?H silylation of several terminal alkynes including two pharmaceuticals. Overall, the presented system allows the synthesis of various attractive silylacetylenes under mild conditions, making this approach an environmentally benign and sustainable alternative to existing synthetic solutions.
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CAS No. : | 23152-99-0 | MDL No. : | MFCD03839988 |
Formula : | C11H12 | Boiling Point : | - |
Linear Structure Formula : | (CH3)2CHC6H4CCH | InChI Key : | CODCGGILXPHCLE-UHFFFAOYSA-N |
M.W : | 144.21 | Pubchem ID : | 637501 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | 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 |
---|---|---|
11.40 g (87%) | dichlorobis(triphenylphosphine)palladium[II]; copper(I) iodide; In triethylamine; | The crude 4-isopropylphenylacetylene was dissolved in triethylamine (100 mL). 4-iodoisopropylbenzene (12.3 g, 50 mmol), dichlorobis(triphenylphosphine)palladium(II) (0.70 g, 1 mmol), and copper(I) iodide (1.5 g) were added. The reaction was stirred at room temperature for 2 days, heated to reflux for 1 hour, cooled, diluted with hexanes, and filtered. The filtrate was evaporated under reduced pressure. The residue was filtered through a pad of silica gel with hexanes, and the solvent was evaporated to give 11.40 g (87%) of 1,2-bis(4-(2-propyl)phenyl)acetylene. |
Yield | Reaction Conditions | Operation in experiment |
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Example 22 Preparation of N-Hydroxy-N-[4-[4-(1-methylethyl)phenyl]-3-butyn-2-yl]urea The title compound was prepared according to the procedure of Example 15 using p-isopropylphenylacetylene instead of p-bromophenylacetylene in step (a), and using trimethylsilyl isocyanate instead of methyl isocyanate in step (d). m.p. 154-156 C.; NMR (300 MHz, DMSO-d6), 1.18 (6H, d, J=7 Hz), 1.35 (3H, d, J=7 Hz), 2.89 (1H, m), 5.12 (1H, q, J=7 Hz), 6.55 (2H, s), 7.22 (2H, d, J=7 Hz), 7.31 (2H, d, J=7 Hz), 9.31 (1H, s); MS (M+1)+ 247, (M+NH4)+ 264. Analysis calc'd for C14 H18 N2 O2: C, 68.26; H, 7.36; N, 11.37. Found: C, 67.80, H, 7.27; N, 11.17. |
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