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CAS No. : | 181696-35-5 | MDL No. : | MFCD26743607 |
Formula : | C16H13NO4S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | LLWOSCPRJRUVST-UHFFFAOYSA-N |
M.W : | 315.34 | Pubchem ID : | 11565904 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
91.4% | Stage #1: With thionyl chloride In dichloromethane at 0 - 5℃; for 0.666667 h; Stage #2: With ammonium hydroxide In dichloromethane at 20℃; for 1 h; |
5-methyl-3-phenyl-4- (4-sulfonic acid phenyl) isoxazole 11.7g (50mmol) dissolved in dichloromethaneOf thionyl chloride was added dropwise 9.3g (100mmol) at 0 ~ 5 reaction was stirred 40 minutes,Quenched with ice water, extracted with dichloromethane,Methylene chloride phase directly into the aqueous ammonia,The reaction temperature was raised to 20 deg.] C continued for 1 hourAfter the reaction, dichloromethane extraction,Washed, concentrated,Methanol to obtain 14.4 g of vediloxib,The yield was 91.4percent and the purity was 99.54percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98.9% | With tris[2-phenylpyridinato-C2,N]iridium(III); magnesium oxide; triethylamine In tetrahydrofuran at 25℃; for 0.5 h; Irradiation | 12.1 g (100 mmol) of benzaldehyde oxime21.6 g (110 mmol) of 1- (4-sulfophenyl) propyne,Tris (2-phenylpyridine) iridium (III) 3.3g (5mmol),(80 mmol) of triethylamine and 1.2 g (30 mmol) of magnesium oxide were added to a flask containing 30 ml of THF,25 for 30min,Light emitted by the blue light-emitting diodes,The illumination wavelength was 455 nm.The reaction solution was concentrated, washed with water and then recrystallized from ethanol,Dried to give 31.2 g of 5-methyl-3-phenyl-4- (4-sulfophenyl) isoxazole in a yield of 98.9percentPurity 99.50percent. |
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