Application of diphenylphosphine methyl-substituted calix [4] arene
A technology of diphenylphosphinomethyl and aromatic hydrocarbons, applied in organic compound/hydride/coordination complex catalysts, sulfonamide preparation, organic chemistry, etc., to achieve high catalytic activity, reduce phosphorus pollution, and good stability Effect
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Embodiment 1
[0035] In a 100 mL three-necked bottle, add N -Benzylidene-4-methylbenzenesulfonimide 12.95 g (50 mmol), methyl vinyl ketone 7.00 g (100 mmol), catalyst diphenylphosphinomethyl-substituted calix[4]arene 4.23 g (5 mmol), 26 g of dichloromethane, stirred at 20°C for 58 h, TLC tracking showed that the reaction of the raw materials was complete. Add 120 g of dichloromethane, wash with saturated brine (30 mL×2), dry the organic phase over anhydrous sodium sulfate and concentrate in vacuo, add 10 g of cold methanol, a solid precipitates, filter to obtain the catalyst, and weigh after drying to obtain 3.47 g, the recovery rate was 82%; after the filtrate was concentrated, it was separated by column chromatography, using petroleum ether / ethyl acetate=4:1 (v / v) as the eluent, and detected by TLC. The eluent of the product, the eluent is distilled to remove the eluent to obtain the aza-Baylis-Hillman adduct 4-methyl- N -(2-Methylene-3-oxo-1-phenylbutyl)benzenesulfonamide, white solid,...
Embodiment 2
[0037] In a 100 mL three-necked bottle, add N -Benzylidene-4-methylbenzenesulfonimide 12.95 g (50 mmol), methyl vinyl ketone 4.20 g (60 mmol), catalyst diphenylphosphinomethyl-substituted calix[4]arene 0.42 g (0.5 mmol), 38 g of ethanol, stirred at 40 °C for 43 h, TLC tracking showed that the reaction of the raw materials was complete. Add 26 g of ethyl acetate for extraction, wash with saturated brine (30 mL×2), dry the organic phase over anhydrous sodium sulfate and concentrate in vacuo, add 1.68 g of cold methanol, a solid precipitates, filter to obtain the catalyst, dry and weigh 0.37 g was obtained, and the recovery rate was 89%; the filtrate was concentrated and separated by column chromatography, using petroleum ether / ethyl acetate=4:1 (v / v) as the eluent, detected by TLC, and collected the aza-Baylis-Hillman plus The eluent of the product, the eluent is distilled to remove the eluent to obtain the aza-Baylis-Hillman adduct 4-methyl- N -(2-Methylene-3-oxo-1-phenylbuty...
Embodiment 3
[0039] In a 100 mL three-necked bottle, add N -Benzylidene-4-methylbenzenesulfonimide 12.95 g (50 mmol), methyl vinyl ketone 10.50 g (150 mmol), catalyst diphenylphosphinomethyl-substituted calix[4]arene 21.17 g (25 mmol), 48 g of ethyl acetate, stirred at 15°C for 50 h, and TLC tracking showed that the reaction of the raw materials was complete. Add 130 g of diethyl ether for extraction, wash with saturated brine (30 mL×2), dry the organic phase with anhydrous sodium sulfate and concentrate in vacuo, add 21.17 g of cold methanol, a solid precipitates, filter to obtain the catalyst, and weigh after drying to obtain 15.88 g, the recovery rate was 75%; the filtrate was concentrated and separated by column chromatography, using petroleum ether / ethyl acetate = 4:1 (v / v) as the eluent, and detected by TLC, the collection contained aza-Baylis-Hillman The eluent of the product, the eluent is distilled to remove the eluent to obtain the aza-Baylis-Hillman adduct 4-methyl- N -(2-Meth...
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