反应 #4034697
相关文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-0801e519da424e8981d3d835fd15feb0暂无可渲染的结构数据
CCOC(=O)CC1(CCOCC1)O产品信息
乙基 2-(4-羟基氧杂-4-基)乙酸甲酯(CAS 401811-99-2)的产品身份、结构标识及相关反应资料,供化学中间体检索、研发和采购评估使用。
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12 条反应 · 12 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-0801e519da424e8981d3d835fd15feb0反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-c75e31060f3d41719836347a76ac2e64反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of ethyl(4-hydroxytetrahydro-2H-pyran-4-yl)acetate (6.73 g, 35.8 mmol) and benzonitrile (4.05 ml, 39.3 mmol) was added conc. sulfuric acid (25 ml) under ice-cooling. After stirring at room temperature for 16 hrs., the reaction mixture was added to water (100 ml) under ice-cooling, and the mixture was extracted with ethyl acetate. The extract washed with saturated aqueous sodium hydrogen carbonate solution, then with saturated brine and dried over anhydrous MgSO4. After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue, and the mixture was heated under reflux for 6 hrs. Water (200 ml) was added to the reaction mixture and the mixture was washed with diethyl ether. The aqueous layer was acidified (pH 2) with 5N hydrochloric acid, extracted with ethyl acetate-tetrahydrofuran (2:1, v/v). The extract was washed with saturated brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The obtained solid was collected by filtration and washed with diisopropyl ether to give the title compound (1.64 g, 17%) as colorless crystals. cooling cooling the mixture was extracted with ethyl acetate The extract washed with saturated aqueous sodium hydrogen carbonate solution with saturated brine and dried over anhydrous MgSO4 After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue the mixture was heated under reflux for 6 hrs Water (200 ml) was added to the reaction mixture the mixture was washed with diethyl ether extracted with ethyl acetate-tetrahydrofuran (2:1 The extract was washed with saturated brine dried over anhydrous Na2SO4 concentrated under reduced pressure The obtained solid was collected by filtration washed with diisopropyl ether
来源 ID: ord-8c320cdedddb44a18dd3d862cbc92fd7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of ethyl(4-hydroxytetrahydro-2H-pyran-4-yl)acetate (6.73 g, 35.8 mmol) and benzonitrile (4.05 ml, 39.3 mmol) was added conc. sulfuric acid (25 ml) under ice-cooling. After stirring at room temperature for 16 hrs., the reaction mixture was added to water (100 ml) under ice-cooling, and the mixture was extracted with ethyl acetate. The extract washed with saturated aqueous sodium hydrogen carbonate solution, then with saturated brine and dried over anhydrous MgSO4. After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue, and the mixture was heated under reflux for 6 hrs. Water (200 ml) was added to the reaction mixture and the mixture was washed with diethyl ether. The aqueous layer was acidified (pH 2) with 5N hydrochloric acid, extracted with ethyl acetate-tetrahydrofuran (2:1, v/v). The extract was washed with saturated brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The obtained solid was collected by filtration and washed with diisopropyl ether to give the title compound (1.64 g, 17%) as colorless crystals. cooling cooling the mixture was extracted with ethyl acetate The extract washed with saturated aqueous sodium hydrogen carbonate solution with saturated brine and dried over anhydrous MgSO4 After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue the mixture was heated under reflux for 6 hrs Water (200 ml) was added to the reaction mixture the mixture was washed with diethyl ether extracted with ethyl acetate-tetrahydrofuran (2:1 The extract was washed with saturated brine dried over anhydrous Na2SO4 concentrated under reduced pressure The obtained solid was collected by filtration washed with diisopropyl ether
来源 ID: ord-8c320cdedddb44a18dd3d862cbc92fd7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of tetrahydro-4H-pyran-4-one (5.5 g, 51.6 mmol), a zinc powder (4.05 g, 61.9 mmol) and a small amount of iodine in tetrahydrofuran (60 ml) was added dropwise ethyl bromoacetate (6.28 ml, 56.7 mmol) under a nitrogen atmosphere. After heating under reflux for 6 hrs., 10% sulfuric acid (50 ml) was carefully added under ice-cooling and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous MgSO4 and concentrated under reduced pressure to give the title compound (6.73 g, 69%) as a colorless oil. After heating under reflux for 6 hrs cooling the mixture was extracted with ethyl acetate The extract was washed with saturated aqueous sodium hydrogen carbonate solution dried over anhydrous MgSO4 concentrated under reduced pressure
来源 ID: ord-79c693d83c034df8ab33ca7eea5732a6反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of ethyl (4-hydroxytetrahydro-2H-pyran-4-yl)acetate (6.73 g, 35.8 mmol) and benzonitrile (4.05 ml, 39.3 mmol) was added conc. sulfuric acid (25 ml) under ice-cooling. After stirring at room temperature for 16 hrs., the reaction mixture was added to water (100 ml) under ice-cooling, and the mixture was extracted with ethyl acetate. The extract washed with saturated aqueous sodium hydrogen carbonate solution, then with saturated brine and dried over anhydrous MgSO4. After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue, and the mixture was heated under reflux for 6 hrs. Water (200 ml) was added to the reaction mixture and the mixture was washed with diethyl ether. The aqueous layer was acidified (pH 2) with 5N hydrochloric acid, extracted with ethyl acetate-tetrahydrofuran (2:1, v/v). The extract was washed with saturated brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The obtained solid was collected by filtration and washed with diisopropy ether to give the title compound (1.64 g, 17%) as colorless crystals. cooling cooling the mixture was extracted with ethyl acetate The extract washed with saturated aqueous sodium hydrogen carbonate solution with saturated brine and dried over anhydrous MgSO4 After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue the mixture was heated under reflux for 6 hrs Water (200 ml) was added to the reaction mixture the mixture was washed with diethyl ether extracted with ethyl acetate-tetrahydrofuran (2:1 The extract was washed with saturated brine dried over anhydrous Na2SO4 concentrated under reduced pressure The obtained solid was collected by filtration washed with diisopropy ether
来源 ID: ord-d6b799152dc54fceadee54935d3e079b反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of tetrahydro-4H-pyran-4-one (5.5 g, 51.6 mmol), a zinc powder (4.05 g, 61.9 mmol) and a small amount of iodine in tetrahydrofuran (60 ml) was added dropwise ethyl bromoacetate (6.28 ml, 56.7 mmol) under a nitrogen atmosphere. After heating under reflux for 6 hrs., 10% sulfuric acid (50 ml) was carefully added under ice-cooling and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous MgSO4 and concentrated under reduced pressure to give the title compound (6.73 g, 69%) as a colorless oil. After heating under reflux for 6 hrs cooling the mixture was extracted with ethyl acetate The extract was washed with saturated aqueous sodium hydrogen carbonate solution dried over anhydrous MgSO4 concentrated under reduced pressure
来源 ID: ord-ccb328de8a8c4417bd2588f7bb8262d5反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of ethyl (4-hydroxytetrahydro-2H-pyran-4-yl)acetate (6.73 g, 35.8 mmol) and benzonitrile (4.05 ml, 39.3 mmol) was added conc. sulfuric acid (25 ml) under ice-cooling. After stirring at room temperature for 16 hrs., the reaction mixture was added to water (100 ml) under ice-cooling, and the mixture was extracted with ethyl acetate. The extract washed with saturated aqueous sodium hydrogen carbonate solution, then with saturated brine and dried over anhydrous MgSO4. After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue, and the mixture was heated under reflux for 6 hrs. Water (200 ml) was added to the reaction mixture and the mixture was washed with diethyl ether. The aqueous layer was acidified (pH 2) with 5N hydrochloric acid, extracted with ethyl acetate-tetrahydrofuran (2:1, v/v). The extract was washed with saturated brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The obtained solid was collected by filtration and washed with diisopropy ether to give the title compound (1.64 g, 17%) as colorless crystals. cooling cooling the mixture was extracted with ethyl acetate The extract washed with saturated aqueous sodium hydrogen carbonate solution with saturated brine and dried over anhydrous MgSO4 After concentration under reduced pressure, ethanol (50 ml) and 50% aqueous potassium hydroxide solution (10 ml) was added to the obtained residue the mixture was heated under reflux for 6 hrs Water (200 ml) was added to the reaction mixture the mixture was washed with diethyl ether extracted with ethyl acetate-tetrahydrofuran (2:1 The extract was washed with saturated brine dried over anhydrous Na2SO4 concentrated under reduced pressure The obtained solid was collected by filtration washed with diisopropy ether
来源 ID: ord-81dbf11d00784b7c9dc0ce5a84820c9c反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of tetrahydro-4H-pyran-4-one (5.5 g, 51.6 mmol), a zinc powder (4.05 g, 61.9 mmol) and a small amount of iodine in tetrahydrofuran (60 ml) was added dropwise ethyl bromoacetate (6.28 ml, 56.7 mmol) under a nitrogen atmosphere. After heating under reflux for 6 hrs., 10% sulfuric acid (50 ml) was carefully added under ice-cooling and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous MgSO4 and concentrated under reduced pressure to give the title compound (6.73 g, 69%) as a colorless oil. After heating under reflux for 6 hrs cooling the mixture was extracted with ethyl acetate The extract was washed with saturated aqueous sodium hydrogen carbonate solution dried over anhydrous MgSO4 concentrated under reduced pressure
来源 ID: ord-4cb1496c2e9c4a728e8e5e5e96511a7c反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of tetrahydro-4H-pyran-4-one (5.5 g, 51.6 mmol), a zinc powder (4.05 g, 61.9 mmol) and a small amount of iodine in tetrahydrofuran (60 ml) was added dropwise ethyl bromoacetate (6.28 ml, 56.7 mmol) under a nitrogen atmosphere. After heating under reflux for 6 hrs., 10% sulfuric acid (50 ml) was carefully added under ice-cooling and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous MgSO4 and concentrated under reduced pressure to give the title compound (6.73 g, 69%) as a colorless oil. After heating under reflux for 6 hrs cooling the mixture was extracted with ethyl acetate The extract was washed with saturated aqueous sodium hydrogen carbonate solution dried over anhydrous MgSO4 concentrated under reduced pressure
来源 ID: ord-4cb1496c2e9c4a728e8e5e5e96511a7c反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-0801e519da424e8981d3d835fd15feb0反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-c75e31060f3d41719836347a76ac2e64PubChem References
以下资料来自该化合物的公开数据库参考记录。
