A method for the highly selective reduction of alkynes to z-type alkenes
A synthesis method and olefin technology, applied in the field of organic compound synthesis, can solve problems such as few researches
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Embodiment 1
[0032]
[0033] 0.02 mmol chloride (2 mg), 0.03 mmol 1,3-bis (2,4,6-trimethyl) chlorinated (10.3 mg), 0.2 mmol of tert-butoxide (22.4 mg) In the Schlenk reaction tube, the vacuum was evacuated, and the nitrogen was charged 3 times, 1 ml of ethanol was added as a solvent, and stirred at room temperature for 15 min. 0.2 mmol of diphenyl acetylene (35.6 mg) and 0.24 mmol of boronic acid-cell acid-torubol ester (61 mg) were added to 2 ml of ethanol, and then added dropwise to the reaction tube, and the reaction was stirred at room temperature for 5 hours. After the reaction, 100-200 mesh chromatographic silica gel was added to the obtained reaction mixture and the solvent was evaporated to remove the resulting crude product, and the obtained crude product was separated, and the volume ratio of 50: 1 petroleum ether and acetate The mixture of esters is eluted as the eluent, and the TLC tracks the elution process, and the eluent containing the target product is collected, and the elue...
Embodiment 2
[0036]
[0037] 0.01 mmol of chloride (1 mg), 0.02 mmol 1,3-bis (2,4,6-trimethylphenyl) chlorinated (6.9 mg), 0.2 mmol of tert-butoxide (22.4 mg) In the Schlenk reaction tube, the vacuum was evacuated, and the nitrogen was charged 3 times, 1 ml of ethanol was added as a solvent, and stirred at room temperature for 15 min. 0.2 mmol of diphenyl acetylene (35.6 mg) and 0.24 mmol of boric acid-ravate (61 mg) were dissolved in 2 ml of ethanol, and then added to the reaction tube, and the mixture was stirred at room temperature for 5 hours. After the reaction, 100-200 mesh chromatographic silica gel was added to the obtained reaction mixture and the solvent was evaporated to remove the resulting crude product, and the obtained crude product was separated, and the volume ratio of 50: 1 petroleum ether and acetate The mixture of esters is eluted as the eluent, and the TLC tracks the elution process, and the eluent containing the target product is collected, and the eluent is evaporated ...
Embodiment 3
[0040]
[0041] 0.005 mmol chloride (0.5 mm), 0.01 mmol 1,3-bis (2,4,6-trimethylphenyl) chlorosolium chlorolium (3.4 mg), 0.2 mmol of tert-butoxide (22.4 mg) Add the Schlenk reaction tube, evacuate, and then charge 3 times, 1 ml of ethanol is added as a solvent, and stirred at room temperature for 15 min. 0.2 mmol of diphenyl acetylene (35.6 mg) and 0.24 mmol of boric acid-ravate (61 mg) were dissolved in 2 ml of ethanol, and then added to the reaction tube, and the mixture was stirred at room temperature for 5 hours. After the reaction, 100-200 mesh chromatographic silica gel was added to the obtained reaction mixture and the solvent was evaporated to remove the resulting crude product, and the obtained crude product was separated, and the volume ratio of 50: 1 petroleum ether and acetate The mixture of esters is eluted as the eluent, and the TLC tracks the elution process, and the eluent containing the target product is collected, and the eluent is evaporated to evaporase to o...
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