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With tetrabutylammomium bromide; caesium carbonate; In tert-butyl methyl ether; at 50℃; |
At room temperature, Biphenylmethylene glycine ethyl ester(1A) (50 g, 0.187 mol) was dissolved in methyl t-butyl ether (300 mL)A mixture of <strong>[6165-75-9]propargyl benzenesulfonate</strong> (44 g, 0.224 mol)Tetrabutylammonium bromide (6.1 g, 0.019 mol) was added to the reaction solution, the temperature was raised to 50 °C, cesium carbonate (121.8 g, 0.374 mol) was added and reacted at 50° C overnight. The reaction solution was filtered, the filter cake was washed with methyl t-butyl ether (40 mL x 2), the organic phases were combined, concentrated to half volume by rotary evaporation, hydrochloric acid solution (3 mol / L, 100 mL) was added and stirred at room temperature for 1 hour , Static stratification,The aqueous phase was extracted with methyl t-butyl ether (70 mL x 2) and the aqueous phase was collected to afford 1B. |
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With tetrabutylammomium bromide; caesium carbonate; In tert-butyl methyl ether; at 20 - 50℃; |
At room temperature, the dibenzylidene glycine ethyl ester 1A(50g, 0.187 muM) soluble in methyl tert-butyl ether (300 ml), propargylbenzene sulfonate (44g, 0.224 muM), tetrabutyl ammonium bromide (6.1g, 0.019 muM) is added to the reaction solution, heating to 50 °C, adding cesium carbonate (121.8g, 0.374 muM), 50 °C temperature for the reaction overnight. The reaction liquid filtering, methyl tert-butyl ether for 3rd (40mL × 2) washing the filter cake, combined with the organic phase, the rotary evaporating concentrated to half-volume, adding hydrochloric acid solution (3 mol/L, 100 ml), stirring at room temperature 1 hour, layered, 3rd phase for methyl tert-butyl ether (70mL × 2) extraction, collection of the water phase, to obtain1B. |
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With tetrabutylammomium bromide; caesium carbonate; In tert-butyl methyl ether; at 50℃; |
At room temperature,The diphenylmethylene glycine ethyl ester 1A (50 g, 0.187 mol) Was dissolved in methyl tertiary butyl ether (300 mL)Join Propargylbenzenesulfonate (44 g, 0.224 mol)And tetrabutylammonium bromide (6.1 g, 0.019 mol)The temperature was raised to 50 ° C, cesium carbonate (121.8 g, 0.374 mol)The reaction was carried out at 50 ° C overnight. The reaction solution was filtered,The filter cake was washed with methyl tertiary butyl ether (40 mL x 2), the organic phases were combined, the mixture was concentrated to half volume, hydrochloric acid solution (3 mol / L, 100 mL) was added, stirred at room temperature for 1 hour, The aqueous phase was extracted with methyl tertiary butyl ether (70 mL x 2), the aqueous phase was collected and concentrated to afford 1B. |
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With tetrabutylammomium bromide; caesium carbonate; In tert-butyl methyl ether; at 50℃; |
At room temperature,A solution of 1A (50 g, 0.187 mol) in methyl tert-butyl ether (300 mL)Add <strong>[6165-75-9]propargylbenzenesulfonate</strong>(44 g, 0.224 mol)And tetrabutylammonium bromide (6.1 g, 0.019 mol)The temperature was raised to 50 ° C, cesium carbonate (121.8 g,0.374 mol),The reaction was carried out at 50 ° C overnight.The reaction solution was filtered,The filter cake was washed with methyl tert-butyl ether (40 mL x 2)Combined organic phase,Steamed to half volume,A solution of hydrochloric acid (3 mol / L, 100 mL) was added,The mixture was stirred at room temperature for 1 hour,Static liquid separation,The aqueous phase was extracted with methyl tert-butyl ether (70 mL x 2)Collecting water,Concentrated to get 1B. |
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With tetrabutylammomium bromide; caesium carbonate; In tert-butyl methyl ether; at 50℃; |
Diphenylmethylene glycine ethyl ester 1A (50 g, 0.187 mol) at room temperatureSoluble in methyl tert-butyl ether (300 mL),Propargyl besylate (44 g, 0.224 mol),Tetrabutylammonium bromide (6.1 g, 0.019 mol) was added to the reaction solution.Warming up to 50 ° C,Add cesium carbonate (121.8 g, 0.374 mol),The reaction was carried out overnight at a temperature of 50 °C.The reaction solution was filtered, and the filter cake was washed with methyl t-butyl ether (40 mL×2).Combine the organic phase,After concentrating half a volume of solvent by rotary evaporation,Add hydrochloric acid solution (3mol/L, 100mL),Stir at room temperature for 1 hour, let stand for stratification.The aqueous phase was extracted with methyl tert-butyl ether (70 mL x 2).The aqueous phase was collected to obtain 1B. |
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