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With Cu exchanged bentonite In neat (no solvent) at 80℃; for 0.333333 h; Microwave irradiation
General procedure: Method A (MWI): in this study a continuous focusedmicrowave (synthewave 402 apparatus with a max power of300 W) with refluxing and stirring option was used. Thereaction temperature was reached a target temperature after3min then maintained by device until the end of reaction.The temperature was detected by IR sensor.The mixture of the alkene (6 mmol) and the exchangedbentonite 50 mg was irradiated at 150 Watts to reach 80°C,in a quartz reactor ( = 1.8 cm). The temperature was maintainedfor 20 minutes and during that time, EDA (6 mmol) inalkene (6mmol) was added slowly by a syringe during 10min. When the reaction was complete, the crud mixture wasobtained after adding dichloromethane (3x20mL), filtrationand removal of the excess of alkene and solvent. The crudewas analyzed by 1H NMR and then the product is purified byshort-path distillation. The obtained cyclopropane is identifiedby 1H NMR, 13C NMR and mass spectra.
Reference：
[1] Helvetica Chimica Acta, 1995, vol. 78, # 2, p. 459 - 470
[2] Journal of the American Chemical Society, 2002, vol. 124, # 6, p. 978 - 983
[3] Letters in Organic Chemistry, 2016, vol. 13, # 3, p. 217 - 223
ethyl (1S,2R)-2-(acetyloxy)cyclopropane-1-carboxylate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With Cu exchanged bentonite; In neat (no solvent); at 80.0℃; for 0.333333h;Microwave irradiation;
General procedure: Method A (MWI): in this study a continuous focusedmicrowave (synthewave 402 apparatus with a max power of300 W) with refluxing and stirring option was used. Thereaction temperature was reached a target temperature after3min then maintained by device until the end of reaction.The temperature was detected by IR sensor.The mixture of the alkene (6 mmol) and the exchangedbentonite 50 mg was irradiated at 150 Watts to reach 80C,in a quartz reactor ( = 1.8 cm). The temperature was maintainedfor 20 minutes and during that time, EDA (6 mmol) inalkene (6mmol) was added slowly by a syringe during 10min. When the reaction was complete, the crud mixture wasobtained after adding dichloromethane (3x20mL), filtrationand removal of the excess of alkene and solvent. The crudewas analyzed by 1H NMR and then the product is purified byshort-path distillation. The obtained cyclopropane is identifiedby 1H NMR, 13C NMR and mass spectra.
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