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Type | HazMat fee for 500 gram (Estimated) |
Excepted Quantity | USD 0.00 |
Limited Quantity | USD 15-60 |
Inaccessible (Haz class 6.1), Domestic | USD 80+ |
Inaccessible (Haz class 6.1), International | USD 150+ |
Accessible (Haz class 3, 4, 5 or 8), Domestic | USD 100+ |
Accessible (Haz class 3, 4, 5 or 8), International | USD 200+ |
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CAS No. : | 67475-56-3 | MDL No. : | MFCD03618459 |
Formula : | C7H6ClFO3S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | LUEBMKPHZDSPFH-UHFFFAOYSA-N |
M.W : | 224.64 | Pubchem ID : | 2783409 |
Synonyms : |
|
Signal Word: | Danger | Class: | 8 |
Precautionary Statements: | P280-P305+P351+P338-P310 | UN#: | 3261 |
Hazard Statements: | H314 | 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 |
---|---|---|
84.6% | at 0 - 20℃; | l-fluoro-4-methoxybenzene (10.0 g, 0.079mol) was added dropwise to sulfurochloridic acid (31.4ml, 0.474mol) at 00C, The mixture was stirred at room temperature for about 6h, after which it was added dropwise into ice water. The mixture was extracted with CH2Cl2 three times. The combined extracts were washed with brine, dried over sodium sulfate and concentrated in vacuo to give the title product (15.Og, 84.6percentyield).1H NMR (300 MHz, DMSO-d6) δ 3.74 (s, 3H), 6.97 (dd, J= 4.3, 8.9 Hz, IH), 7.13 (dt, J= 3.4, 8.6 Hz, IH), 7.41 (dd, J= 3.3, 8.8 Hz, IH) |
70% | With chlorosulfonic acid In dichloromethane at 0 - 5℃; for 3 h; Inert atmosphere | General procedure: A solution of the respective anisole (175 mmol) in CH2Cl2 (50 mL) was added dropwise to a 0 °C chlorosulfonic acid (100 mL) so as to maintain the reaction temperature below 5 °C. After the addition was complete, the reaction mixture was stirred for 3 h and poured over ice. The organic phase was separated, washes with water, dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by short-path chromatography on silica gel using 10percent ethyl acetate in hexanes as eluent to provide the analytically pure target compound. |
56% | at 25℃; for 3 h; | To a stirred CISO3H (50 mL) was added l-fiuoro-4-methoxy-benzene (10.0 g, 79.4 mmol) dropwise at 25°C. The mixture was stirred at this temperature for 3 hours. The mixture was poured into ice water (200 mL) and extracted with EtOAc (200 mL). The organic layer was wshed with brine (100 mL), dried over Na2S04 and evaporated in vacuum to give 12 g of crude product. The crude was purifed by silica gel column chromatography (PE/EtOAc, 20/1) to give 10.0 g of 5-fluoro-2-methoxy-benzenesulfonyl chloride (yield: 56percent) as yellow oil |
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