丙戊酸钠EP杂质G

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:

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

实验步骤: In a flask equipped with a dropping-funnel were placed 480 g. of distilled dioxan followed by 80 g. (0.432 mol) of tri-n-propylacetamide which was dissolved by stirring. For a period of 20 minutes a current of dry hydrochloric acid gas was passed through the dioxan solution at room-temperature, which represented a total of 100 g of hydrochloric acid gas. At the end of this operation, 88 g (0.86 mol) of freshly distilled butyl nitrite was slowly added over a period of 2 hours through the dropping-funnel. The temperature of the reaction medium rose from 31° to 43°C which necessitated cooling in a water-bath. The solution was then maintained for 2 hours at 85°-90°C. The dioxan was distilled off under a reduced pressure of 20 mm. Hg and a pasty residue obtained at room-temperature. This residue was dissolved in 290 g of a 10% aqueous solution of potassium hydroxide. The aqueous layer was decanted out and extracted twice with 75 g of ethyl ether. The potassium solution was acidified with 118 g of a 36% solution of hydrochloric acid (at 10° /20°C) after which the oily phase was decanted out. The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase and the ethereal extracts were placed together. The ethereal solution was washed twice with 100 g of water and dried for 24 hours over 100 g of anhydrous sodium sulphate. The sodium sulphate was then centrifuged out. The ethyl ether was distilled off under atmospheric pressure and the residue recuperated under 7 mm. Hg. The fraction obtained boiled at 126° to 128°C and crystallized rapidly. In this way, 61 g of crude tri-n-propylacetic acid were obtained, which represents a yield of 76%. The crude product was then dissolved by heating in 75 g of ethyl ether. The ethereal solution was filtered while hot and the filtrate left at a temperature of -30°C for 4 hours. The precipitate which formed was centrifuged out and dried in a desiccator under a reduced pressure of 20 mm. Hg for 6 hours. By this means, 46 g of pure tri-n-propylacetic acid were obtained which represents a yield in pure product of 75.4% and a total yield of 57.3% M.P. 67°C In a flask equipped with a dropping-funnel rose from 31° to 43°C necessitated cooling in a water-bath The solution was then maintained for 2 hours at 85°-90°C The dioxan was distilled off under a reduced pressure of 20 mm. Hg a pasty residue obtained at room-temperature The aqueous layer was decanted out extracted twice with 75 g of ethyl ether was acidified with 118 g of a 36% solution of hydrochloric acid (at 10° /20°C) was decanted out The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase The ethereal solution was washed twice with 100 g of water dried for 24 hours over 100 g of anhydrous sodium sulphate The ethyl ether was distilled off under atmospheric pressure The fraction obtained boiled at 126° to 128°C crystallized rapidly

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

实验步骤: In a flask equipped with a dropping-funnel were placed 480 g. of distilled dioxan followed by 80 g. (0.432 mol) of tri-n-propylacetamide which was dissolved by stirring. For a period of 20 minutes a current of dry hydrochloric acid gas was passed through the dioxan solution at room-temperature, which represented a total of 100 g of hydrochloric acid gas. At the end of this operation, 88 g (0.86 mol) of freshly distilled butyl nitrite was slowly added over a period of 2 hours through the dropping-funnel. The temperature of the reaction medium rose from 31° to 43°C which necessitated cooling in a water-bath. The solution was then maintained for 2 hours at 85°-90°C. The dioxan was distilled off under a reduced pressure of 20 mm. Hg and a pasty residue obtained at room-temperature. This residue was dissolved in 290 g of a 10% aqueous solution of potassium hydroxide. The aqueous layer was decanted out and extracted twice with 75 g of ethyl ether. The potassium solution was acidified with 118 g of a 36% solution of hydrochloric acid (at 10° /20°C) after which the oily phase was decanted out. The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase and the ethereal extracts were placed together. The ethereal solution was washed twice with 100 g of water and dried for 24 hours over 100 g of anhydrous sodium sulphate. The sodium sulphate was then centrifuged out. The ethyl ether was distilled off under atmospheric pressure and the residue recuperated under 7 mm. Hg. The fraction obtained boiled at 126° to 128°C and crystallized rapidly. In this way, 61 g of crude tri-n-propylacetic acid were obtained, which represents a yield of 76%. The crude product was then dissolved by heating in 75 g of ethyl ether. The ethereal solution was filtered while hot and the filtrate left at a temperature of -30°C for 4 hours. The precipitate which formed was centrifuged out and dried in a desiccator under a reduced pressure of 20 mm. Hg for 6 hours. By this means, 46 g of pure tri-n-propylacetic acid were obtained which represents a yield in pure product of 75.4% and a total yield of 57.3% M.P. 67°C In a flask equipped with a dropping-funnel rose from 31° to 43°C necessitated cooling in a water-bath The solution was then maintained for 2 hours at 85°-90°C The dioxan was distilled off under a reduced pressure of 20 mm. Hg a pasty residue obtained at room-temperature The aqueous layer was decanted out extracted twice with 75 g of ethyl ether was acidified with 118 g of a 36% solution of hydrochloric acid (at 10° /20°C) was decanted out The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase The ethereal solution was washed twice with 100 g of water dried for 24 hours over 100 g of anhydrous sodium sulphate The ethyl ether was distilled off under atmospheric pressure The fraction obtained boiled at 126° to 128°C crystallized rapidly

实验步骤: 投料: 向单口瓶中依次加入13g（1.0eq）116610-A，80%浓硫酸水溶液（5V）搅拌，升温至70~75℃，搅拌3h or过夜 GCMS或TLC（PE:EA=3:1,碘薰水显)监测反应进程（过夜反应不完，可以补加80%硫酸水溶液继续反应） 体系反应完全降温至0~5℃，加入(10V)H2O稀释，滴加入10%NaOH水溶液调节PH=9-10,EA萃取一次，合并有机相用饱和食盐水洗涤，无水硫酸钠干燥，减压蒸馏，粗品经柱层析（PE:EA=10:1~8:1）除杂，PE:EA=4:1出产物，得7.82g，纯度99%，定量96.6%（CDCl3 碳酸乙烯酯）

实验步骤: 投料: 加入TM1至80%浓硫酸中搅拌，升至75℃，搅拌3h.\n监测: GCMS或点板（PE:EA=3:1,I2)监测反应进程\n后处理: 降至冰水浴下，加水稀释，加入NaHCO3水溶液调节PH=8-9,EA萃取水相3次，合并有机相用饱和食盐水洗涤，无水硫酸钠干燥，减压蒸馏，粗品经柱层析（PE:EA=3:1）纯化可得产物

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: In a flask equipped with a dropping-funnel were placed 480 g of distilled dioxan followed by 80 g (0.432 mol) of tri-n-propylacetamide which was dissolved by stirring. For a period of 20 minutes a current of dry hydrochloric acid gas was passed through the dioxan solution at room-temperature, which represented a total of 100 g of hydrochloric acid gas. At the end of this operation, 88 g (0.86 mol) of freshly distilled butyl nitrile was slowly added over a period of 2 hours through the dropping-funnel. The temperature of the reaction medium rose from 31 to 43° C which necessitated cooling in a water-bath. The solution was then maintained for 2 hours at 85°-90° C. The dioxan was distilled off under a reduced pressure of 20 mm. Hg and a pasty residue obtained at room-temperature. This residue was dissolved in 290 g of a 10% aqueous solution of potassium hydroxide. The aqueous layer was decanted out and extracted twice with 75 g of ethyl ether. The potassium solution was acidified with 118 g of a 36% solution of hydrochloric acid (at 10/20° C) after which the oily phase was decanted out. The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase and the ethereal extracts were placed together. The ethereal solution was washed twice with 100 g of water and dried for 24 hours over 100 g of anhydrous sodium sulphate. The sodium sulphate was then centrifuged out. The ethyl ether was distilled off under atmospheric pressure and the residue recuperated under 7 mm Hg. The fraction obtained boiled at 126° to 128° C and crystallized rapidly. In this way, 61 g of crude tri-n-propylacetic acid were obtained, which represents a yield of 76%. The crude product was then dissolved by heating in 75 g of ethyl ether. The ethereal solution was filtered while hot and the filtrate left at a temperature of -30° C for 4 hours. The precipitate which formed was centrifuged out and dried in a desiccator under a reduced pressure of 20 mm Hg for 6 hours. By this means, 46 g of pure tri-n-propylacetic acid were obtained which represents a yield in pure product of 75.4% and a total yield of 57.3%. M.P. 67° C. In a flask equipped with a dropping-funnel was dissolved rose from 31 to 43° C necessitated cooling in a water-bath The solution was then maintained for 2 hours at 85°-90° C The dioxan was distilled off under a reduced pressure of 20 mm. Hg a pasty residue obtained at room-temperature The aqueous layer was decanted out extracted twice with 75 g of ethyl ether was acidified with 118 g of a 36% solution of hydrochloric acid (at 10/20° C) was decanted out The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase The ethereal solution was washed twice with 100 g of water dried for 24 hours over 100 g of anhydrous sodium sulphate The ethyl ether was distilled off under atmospheric pressure The fraction obtained boiled at 126° to 128° C crystallized rapidly

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 2-liter flask an 80% aqueous solution of 550 g of sulphuric acid was placed. While stirring, 110 g (0.66 mol) of tri-n-propylacetonitrile were added over a period of 20 minutes and at room-temperature. The temperature of the reaction medium rose to 80° C after which it was brought up to 105°-110° C for 6 hours. The solution was then cooled to 10° C and slowly poured into iced water (1000 g of purified water and 200 g of ice.) A pasty precipitate gradually formed as the solution was added to the iced water. As soon as the operation was finished, the mixture was stirred for 15 minutes and the precipitate centrifuged out and taken up twice in 350 g of ethyl ether. The ethereal solution was first washed twice with 200 g of water containing 10% of sodium bicarbonate and then twice with 250 g of water. The mixture was dried for 24 hours over 125 g of anhydrous sodium sulphate after which the sodium sulphate was centrifuged out. The ether was then eliminated by means of a rotatory evaporator which provided an oil which crystallized into fine needles which were left under vacuum until a constant weight was obtained. By this means, 113 g of crude tri-n-propylacetamide were obtained which represents a yield of 92.6%. The crude product was then dissolved by heating in 150 g of petroleum ether. After dissolution, 1.15 g of CECA WSL black was added and the mixture refluxed for 30 minutes. The black was then filtered off while the mixture was still hot. The filtrate was cooled to -15° C for 3 hours after which the precipitate which formed was centrifuged out and dried for 24 hours in a drying-oven at 40° C under 20 mm. Hg vacuum. In this way, 98.5 g of pure tri-n-propylacetamide were obtained which represents a yield in pure product of 87.1%. M.P. 69° C. rose to 80° C gradually formed as the solution the mixture was stirred for 15 minutes The ethereal solution was first washed twice with 200 g of water containing 10% of sodium bicarbonate The mixture was dried for 24 hours over 125 g of anhydrous sodium sulphate after which the sodium sulphate The ether was then eliminated by means of a rotatory evaporator which provided an oil which crystallized into fine needles which were left under vacuum until a constant weight was obtained

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

实验步骤: In a flask equipped with a dropping-funnel were placed 480 g. of distilled dioxan followed by 80 g. (0.432 mol) of tri-n-propylacetamide which was dissolved by stirring. For a period of 20 minutes a current of dry hydrochloric acid gas was passed through the dioxan solution at room-temperature, which represented a total of 100 g of hydrochloric acid gas. At the end of this operation, 88 g (0.86 mol) of freshly distilled butyl nitrite was slowly added over a period of 2 hours through the dropping-funnel. The temperature of the reaction medium rose from 31° to 43°C which necessitated cooling in a water-bath. The solution was then maintained for 2 hours at 85°-90°C. The dioxan was distilled off under a reduced pressure of 20 mm. Hg and a pasty residue obtained at room-temperature. This residue was dissolved in 290 g of a 10% aqueous solution of potassium hydroxide. The aqueous layer was decanted out and extracted twice with 75 g of ethyl ether. The potassium solution was acidified with 118 g of a 36% solution of hydrochloric acid (at 10° /20°C) after which the oily phase was decanted out. The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase and the ethereal extracts were placed together. The ethereal solution was washed twice with 100 g of water and dried for 24 hours over 100 g of anhydrous sodium sulphate. The sodium sulphate was then centrifuged out. The ethyl ether was distilled off under atmospheric pressure and the residue recuperated under 7 mm. Hg. The fraction obtained boiled at 126° to 128°C and crystallized rapidly. In this way, 61 g of crude tri-n-propylacetic acid were obtained, which represents a yield of 76%. The crude product was then dissolved by heating in 75 g of ethyl ether. The ethereal solution was filtered while hot and the filtrate left at a temperature of -30°C for 4 hours. The precipitate which formed was centrifuged out and dried in a desiccator under a reduced pressure of 20 mm. Hg for 6 hours. By this means, 46 g of pure tri-n-propylacetic acid were obtained which represents a yield in pure product of 75.4% and a total yield of 57.3% M.P. 67°C In a flask equipped with a dropping-funnel rose from 31° to 43°C necessitated cooling in a water-bath The solution was then maintained for 2 hours at 85°-90°C The dioxan was distilled off under a reduced pressure of 20 mm. Hg a pasty residue obtained at room-temperature The aqueous layer was decanted out extracted twice with 75 g of ethyl ether was acidified with 118 g of a 36% solution of hydrochloric acid (at 10° /20°C) was decanted out The aqueous phase was extracted twice with 75 g of ethyl ether after which the oily phase The ethereal solution was washed twice with 100 g of water dried for 24 hours over 100 g of anhydrous sodium sulphate The ethyl ether was distilled off under atmospheric pressure The fraction obtained boiled at 126° to 128°C crystallized rapidly