tert-butyl 2-(2-cyanophenoxy)acetate

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Cyanophenol (107.1 g) is dissolved in acetone (1000 ml) and is added t-butyl bromoacetate (200.0 g). Furthermore, potassium carbonate (141.6 g) is added, and then the reaction solution is heated under reflux for 2 hours. After allowing to cool, the insoluble materials are removed by filtration, and then the insoluble materials are washed with acetone several times. The filtrate and the washing are combined, concentrated under reduced pressure and treated with diisopropyl ether azeotropically. The resulting residue is crystallized from n-hexane-diisopropyl ether (5/1) (600 ml), and then stirred under ice-cooling. The precipitates are collected by filtration, washed with cold n-hexane-diisopropyl ether (10/1) (600 ml) several times and dried to give the title compounds (194.5 g). the reaction solution is heated under reflux for 2 hours to cool the insoluble materials are removed by filtration the insoluble materials are washed with acetone several times concentrated under reduced pressure treated with diisopropyl ether azeotropically The resulting residue is crystallized from n-hexane-diisopropyl ether (5/1) (600 ml) cooling The precipitates are collected by filtration washed with cold n-hexane-diisopropyl ether (10/1) (600 ml) several times dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Cyanophenol (107.1 g) is dissolved in acetone (1000 ml) and thereto is added t-butyl bromoacetate (200.0 g). Potassium carbonate (141.6 g) is added, and the reaction solution is heated under reflux for 2 hours. After allowing to cool, the insoluble materials are removed by filtration, and the insolubles are washed with acetone several times. The filtrate and washings are combined, concentrated under reduced pressure and treated with diisopropyl ether azeotropically. The resulting residue is crystallized from n-hexane-diisopropyl ether (5/1) (600 ml), followed by stirring under ice-cooling. The precipitates are collected by filtration, washed with cold n-hexane-diisopropyl ether (10/1) (600 ml) several times, and dried to give the title compound (194.5 g). the reaction solution is heated under reflux for 2 hours to cool the insoluble materials are removed by filtration the insolubles are washed with acetone several times concentrated under reduced pressure treated with diisopropyl ether azeotropically The resulting residue is crystallized from n-hexane-diisopropyl ether (5/1) (600 ml) cooling The precipitates are collected by filtration washed with cold n-hexane-diisopropyl ether (10/1) (600 ml) several times dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Cyanophenol (107.1 g) is dissolved in acetone (1000 ml) and is added t-butyl bromoacetate (200.0 g). Furthermore, potassium carbonate (141.6 g) is added, and then the reaction solution is heated under reflux for 2 hours. After allowing to cool, the insoluble materials are removed by filtration, and then the insoluble materials are washed with acetone several times. The filtrate and the washing are combined, concentrated under reduced pressure and treated with diisopropyl ether azeotropically. The resulting residue is crystallized from n-hexane-diisopropyl ether (5/1) (600 ml), and then stirred under ice-cooling. The precipitates are collected by filtration, washed with cold n-hexane-diisopropyl ether (10/1) (600 ml) several times and dried to give the title compounds (194.5 g). the reaction solution is heated under reflux for 2 hours to cool the insoluble materials are removed by filtration the insoluble materials are washed with acetone several times concentrated under reduced pressure treated with diisopropyl ether azeotropically The resulting residue is crystallized from n-hexane-diisopropyl ether (5/1) (600 ml) cooling The precipitates are collected by filtration washed with cold n-hexane-diisopropyl ether (10/1) (600 ml) several times dried