Method for preparing p-tert-butyl o-nitrothiophenol
A technology of nitrothiophenol and tert-butyl o-o, which is applied in the field of synthesis of chemical intermediates, and can solve problems such as difficulty in obtaining, high cost of raw materials, and long reaction routes
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Embodiment 1
[0014] Add 10 moles of o-nitrothiophenol to the reactor, maintain zero temperature and keep stirring, slowly add 300 grams of BF 3 / H 3 PO 4 Composite catalyst and 11 moles of isobutene. The reaction time is 4 hours. After completion, the temperature is raised to 70-75° C., and the stirring reaction is continued for 2 hours. After cooling to room temperature, the organic phase and the catalyst phase were separated, and the organic phase was separated and dissolved in 500 ml of toluene. The toluene solution was washed 4 times with 1000 ml of water, and dried over anhydrous magnesium sulfate. The toluene was removed by rotary evaporation, and the residue was distilled under reduced pressure (80-100° C. / 1 mmHg) to obtain the product p-tert-butyl-o-nitrothiophenol with a yield of 70%.
Embodiment 2
[0016] Add 50 grams of o-nitrothiophenol in 250 milliliters of stirring reactors, 10 grams of strongly acidic cationic resins (macroporous styrene-divinylbenzenesulfonic acid type cationic exchange resins), decompress to 200 millimeters of mercury, system Maintaining the reaction temperature at 120°C, 180 ml of tert-butyl methyl ether was added to the reaction kettle within 1 hour. After the completion of the insulation reaction for 2h. Cool to room temperature, add 100ml of dichloromethane to dissolve, wash the organic phase with 20ml of water 4 times, and dry over anhydrous magnesium sulfate. The solvent was removed by rotary evaporation to obtain a crude product of p-tert-butyl-o-nitrothiophenol, and the yield of the crude product was 68%.
Embodiment 3
[0018] Add 10 moles of 4,4'-di-tert-butyl-2,2'-dinitrodiphenyl sulfide to the reactor, maintain zero temperature and keep stirring, slowly add 150 grams of AlCl 3 , 620 g (10.9 moles) of isobutyl chloride. After completion, the temperature was raised to 0-10 degrees and the reaction was stirred for 2 hours. The temperature was raised to 70-75 degrees, and the stirring reaction was continued for 2h. After cooling to room temperature, 500 ml of dichloromethane was added and extracted with 100 ml. The organic phases were combined, washed 4 times with 1000 ml of water, and dried over anhydrous magnesium sulfate. The solvent was removed by rotary evaporation to obtain the crude product of 4,4'-di-tert-butyl-2,2'-dinitrodiphenylsulfide, and the yield of the crude product was 78%.
[0019] Add 20 milliliters of methanol, 6 mmoles of 4,4'-di-tert-butyl-2,2'-dinitrodiphenylsulfide in the reaction flask, 2 Stir and heat to reflux under atmosphere, add dropwise a solution of 0.96 g (...
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