反应 #4155345
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-17b051b36aca43759dbc8057c1279bf7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-17b051b36aca43759dbc8057c1279bf7反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-84c64e5bd3b24afc99878e87023ad595反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-17b051b36aca43759dbc8057c1279bf7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 20 g of 4-aminophenol (Mw=109.13; 0.18324 mol) are suspended in 200 cm3 of anhydrous dichloromethane, under an inert atmosphere. The suspension is cooled to a temperature of 0° C. in a bath of ice and 16.4 cm3 of anhydrous pyridine (Mw=79.10; d=0.981; 0.2034 mol) are then added. 17.6 cm3 of ethyl chloroformate (Mw=108.53; d=1.13; 0.18324 mol) are then added dropwise so as to keep the mixture at a temperature below 10° C. The reaction mixture is kept stirring for two hours. The mixture is poured onto one liter of ice-cold water and then extracted with ethyl acetate. The organic phase is washed with water and then dried, filtered and evaporated under vacuum. After recrystallization from a heptane/ethyl acetate mixture, 21 g of a white powder are obtained, which corresponds to a yield of 63%. The melting point of the product obtained is 127.2° C. The H NMR spectrum and the elemental analysis are in accordance with the expected product. are then added at a temperature below 10° C extracted with ethyl acetate The organic phase is washed with water dried filtered evaporated under vacuum After recrystallization from a heptane/ethyl acetate mixture, 21 g of a white powder are obtained The melting point of the product obtained is 127.2° C
来源 ID: ord-d502408c7d244ed88c70e94eaa82836d反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: p-aminophenol 33.36 g (0.3 mole) and 12 g NaOH were dissolved in 120 ml water and cooled to ice salt bath temperature. To the stirring solution, 24 ml ethylchloroformate were slowly added. A white precipitate was found. One gram sodium dithionite was added and mixed. The solid was filtered by suction and washed with cold water (50 ml). Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°. cooled to ice salt bath temperature mixed The solid was filtered by suction washed with cold water (50 ml) Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°
来源 ID: ord-5f15a18293664558970e03a624f3cec7反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-84c64e5bd3b24afc99878e87023ad595反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: p-aminophenol 33.36 g (0.3 mole) and 12 g NaOH were dissolved in 120 ml water and cooled to ice salt bath temperature. To the stirring solution, 24 ml ethylchloroformate were slowly added. A white precipitate was found. One gram sodium dithionite was added and mixed. The solid was filtered by suction and washed with cold water (50 ml). Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°. cooled to ice salt bath temperature mixed The solid was filtered by suction washed with cold water (50 ml) Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°
来源 ID: ord-6649b85c5e514d73833e96c69d40f29f反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: p-aminophenol 33.36 g (0.3 mole) and 12 g NaOH were dissolved in 120 ml water and cooled to ice salt bath temperature. To the stirring solution, 24 ml ethylchloroformate were slowly added. A white precipitate was found. One gram sodium dithionite was added and mixed. The solid was filtered by suction and washed with cold water (50 ml). Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°. cooled to ice salt bath temperature mixed The solid was filtered by suction washed with cold water (50 ml) Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°
来源 ID: ord-6649b85c5e514d73833e96c69d40f29f反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: p-aminophenol 33.36 g (0.3 mole) and 12 g NaOH were dissolved in 120 ml water and cooled to ice salt bath temperature. To the stirring solution, 24 ml ethylchloroformate were slowly added. A white precipitate was found. One gram sodium dithionite was added and mixed. The solid was filtered by suction and washed with cold water (50 ml). Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°. cooled to ice salt bath temperature mixed The solid was filtered by suction washed with cold water (50 ml) Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°
来源 ID: ord-9c8be16579e44df7a80ecc209edf1a82反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: p-aminophenol 33.36 g (0.3 mole) and 12 g NaOH were dissolved in 120 ml water and cooled to ice salt bath temperature. To the stirring solution, 24 ml ethylchloroformate were slowly added. A white precipitate was found. One gram sodium dithionite was added and mixed. The solid was filtered by suction and washed with cold water (50 ml). Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°. cooled to ice salt bath temperature mixed The solid was filtered by suction washed with cold water (50 ml) Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°
来源 ID: ord-9c8be16579e44df7a80ecc209edf1a82反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: p-aminophenol 33.36 g (0.3 mole) and 12 g NaOH were dissolved in 120 ml water and cooled to ice salt bath temperature. To the stirring solution, 24 ml ethylchloroformate were slowly added. A white precipitate was found. One gram sodium dithionite was added and mixed. The solid was filtered by suction and washed with cold water (50 ml). Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°. cooled to ice salt bath temperature mixed The solid was filtered by suction washed with cold water (50 ml) Recrystallization from hot water gave a crystalline powder, 48.3 g (89%), MP 120°-123°
来源 ID: ord-9c8be16579e44df7a80ecc209edf1a82反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 20 g of 4-aminophenol (Mw=109.13; 0.18324 mol) are suspended in 200 cm3 of anhydrous dichloromethane, under an inert atmosphere. The suspension is cooled to a temperature of 0° C. in a bath of ice and 16.4 cm3 of anhydrous pyridine (Mw=79.10; d=0.981; 0.2034 mol) are then added. 17.6 cm3 of ethyl chloroformate (Mw=108.53; d=1.13; 0.18324 mol) are then added dropwise so as to keep the mixture at a temperature below 10° C. The reaction mixture is kept stirring for two hours. The mixture is poured onto one litre of ice-cold water and then extracted with ethyl acetate. The organic phase is washed with water and then dried, filtered and evaporated under vacuum. After recrystallization from a heptane/ethyl acetate mixture, 21 g of a white powder are obtained, which corresponds to a yield of 63%. The melting point of the product obtained is 127.2° C. The 1H NMR spectrum and the elemental analysis are in accordance with the expected product. are then added at a temperature below 10° C extracted with ethyl acetate The organic phase is washed with water dried filtered evaporated under vacuum After recrystallization from a heptane/ethyl acetate mixture, 21 g of a white powder are obtained The melting point of the product obtained is 127.2° C
来源 ID: ord-a0e8deff1dd34a2c87c6b75545d973ffPubChem References
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