One-step preparation method of 2-tert-butyl-5-methoxy isoindoline-1,3-diketone with imine as starting material
A technology based on methoxyisoindoline and tert-butyl, which is applied in the fields of medicine, life science and biology, can solve the problems of poor separation effect and low yield, achieve excellent yield, mild reaction conditions, and improve application value Effect
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Embodiment 1
[0023] In a 25mL test tube, add (E)-N-tert-butyl-1-(4-methoxyphenyl)methanimine 0.2 mmol, dichlorodiacetonitrile palladium 0.01 mmol, copper oxide 0.2 mmol, add Toluene and N,N-dimethylformamide were used as a mixed solvent with a volume ratio of 10:1, 0.2 mmol of water was added, and then a balloon containing carbon monoxide and oxygen was used as a carbonyl source, and stirred at 100 degrees Celsius for 24 hours. After the TLC (thin layer chromatography) detection reaction, the reaction solution was cooled to room temperature, the balloon was removed, and the unreacted carbon monoxide and oxygen were slowly vented. The reaction solution was filtered, the filtrate was evaporated under reduced pressure to remove the solvent, and then separated and purified by column chromatography to obtain the target product 2-tert-butyl-5-methoxyisoindoline-1,3-dione. The column layer used The eluent was a mixed solvent of petroleum ether:ethyl acetate with a volume ratio of 10:1, and the yi...
Embodiment 2
[0026] In a 25mL test tube, add (E)-N-tert-butyl-1-(4-methoxyphenyl)methanimine 0.2 mmol, dichlorodiacetonitrile palladium 0.01 mmol, copper oxide 0.2 mmol, add Toluene was used as a solvent, 0.2 mmol of water was added, and then a balloon containing carbon monoxide and oxygen was covered as a carbonyl source, and stirred at 100 degrees Celsius for 24 hours. TLC (thin layer chromatography) tracking detection, no target product was detected.
Embodiment 3
[0028] In a 25mL test tube, add (E)-N-tert-butyl-1-(4-methoxyphenyl)methanimine 0.2 mmol, dichlorodiacetonitrile palladium 0.01 mmol, copper oxide 0.2 mmol, add N,N-dimethylformamide was used as a solvent, 0.2 mmol of water was added, and then a balloon containing carbon monoxide and oxygen was used as a carbonyl source, and stirred at 100 degrees Celsius for 24 hours. TLC (thin layer chromatography) tracking detection, no target product was detected.
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