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CAS No. : | 43141-66-8 | MDL No. : | MFCD20486161 |
Formula : | C7H5ClF2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | N/A |
M.W : | 162.56 | Pubchem ID : | 640451 |
Synonyms : |
|
TPSA :Topological Polar Surface Area | 0 | H-Bond Acceptor Count : | 2 |
XLogP3 : | - | H-Bond Donor Count : | 0 |
SP3 : | 0.14 | Rotatable Bond Count : | 1 |
Signal Word: | Warning | Class | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H227-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80 %Spectr. | With tris-(dibenzylideneacetone)dipalladium(0); potassium carbonate; hydroquinone; [5-(diphenylphosphanyl)-9,9-dimethyl-9H-xanthen-4-yl]diphenylphosphane In 1,4-dioxane at 110℃; for 48.00 h; Inert atmosphere; Sealed tube | General procedure: To a 25 ml sealed tube were added anhydrous K2CO3 (powder, 4.0 equiv.), hydroquinone (2.0 equiv.), Pd2(dba)3 (2.5 molpercent), Xantphos (7.5 molpercent) and ArB(OH)2 (0.3 or 0.5 mmol) or Ar-Beg (0.3 or 0.5 mmol) under argon. A solution of ClCF2H in 1,4-dioxane (2.0 M, 1.5 ml for 0.3 mmol scale or 2.5 ml for 0.5 mmol scale, 10 equiv.) and fresh distilled 1,4-dioxane (1.0 ml for 0.3 mmol scale or 2.5 ml for 0.5 mmol scale) were added subsequently. The sealed tube was screw capped and heated to 110 °C (oil bath). After stirring for 48 h, the reaction was cooled to room temperature and fluorobenzene (1.0 equiv.) was added. The yield was determined by 19F NMR before working up. The reaction mixture was then diluted with ethyl acetate, filtered through a pad of Celite and concentrated. The residue was purified with silica gel chromatography to provide the desired product. |
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