反应 #4172269
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-54a09e2abc85487f9559e2a95603970c暂无可渲染的结构数据
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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-54a09e2abc85487f9559e2a95603970c反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-ceae3e3154bf40bab8878878bdc313c0反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-54a09e2abc85487f9559e2a95603970c反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-51eced5a435444eeba42ffd4adbf1420反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-51eced5a435444eeba42ffd4adbf1420反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-9a75a0960f6d4dac9a13d4dd7bfc16cb反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-da6fedaf49bb44f0a01d1ff0ecf5e09e反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-ceae3e3154bf40bab8878878bdc313c0反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-da6fedaf49bb44f0a01d1ff0ecf5e09e反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-51eced5a435444eeba42ffd4adbf1420反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-9a75a0960f6d4dac9a13d4dd7bfc16cb反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°. to rise to a maximum of +10° Stirring of the mixture is then continued at 20° the resulting precipitate is suction-filtered washed with ether The filtrate is concentrated by evaporation in vacuo the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours whilst cooling with ice The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered washed with water and ether dried in vacuo
来源 ID: ord-da6fedaf49bb44f0a01d1ff0ecf5e09ePubChem References
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