反应 #4014282
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openreactiondata ↗doi:10.1039/C8SC04228D
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-1f90aeeb035a4412a15a084befb798d5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-1f90aeeb035a4412a15a084befb798d5反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 23.3 g (0.2 mol+10% excess) of the sodium salt of acetylcyanamide and 30.5 g (0.2 mol) of vinylbenzyl chloride (technical mixture of isomers containing approx. 40% of the para-component and 60% of the meta-component) are reacted in 100 ml of dimethylformamide for 8 hours at 48°-50° C., when the reaction is complete the mixture is filtered with suction, the filtrate is introduced into 300 g of ice and 500 ml of water while stirring vigorously and the mixture is then extracted with ethyl acetate. The ethyl acetate solution is dried with anhydrous sodium sulfate and filtered with suction, the filtrate is decolourised with active charcoal, the solution is filtered and the filtrate is concentrated in vacuo at 40° C. on a rotary evaporator. The residue is dried to constant weight at 40° C./0.13 mbar. This gives 34.9 g (87.1% of theory) of a brownish, viscous liquid, which is purified by bulb tube distillation at 130°-145° C./0.7 mbar. containing approx. 40% of the para-component and 60% of the meta-component) is filtered with suction the filtrate is introduced into 300 g of ice and 500 ml of water the mixture is then extracted with ethyl acetate The ethyl acetate solution is dried with anhydrous sodium sulfate filtered with suction the solution is filtered the filtrate is concentrated in vacuo at 40° C. on a rotary evaporator The residue is dried to constant weight at 40° C./0.13 mbar This gives 34.9 g (87.1% of theory) of a brownish, viscous liquid, which is purified by bulb tube distillation at 130°-145° C./0.7 mbar
来源 ID: ord-5935d9e88c544478962797d5696cf3e5反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a 250 mL flask was added vinylbenzyl chloride (7.63 g, 0.050 mol), concentrated aqueous ammonia (9.8 mL), and isopropanol (40 mL). The mixture was stirred for one week, at which point a large quantity of crystalline material (ammonium chloride) had precipitated. The solid was filtered off and washed with isopropanol. The mother liquor was evaporated on a rotary evaporator until no ammonia odor could be detected. Isopropanol (50 mL) was then added, and the mixture refrigerated for several hours. Following refrigeration, ammonium chloride which had precipitated was filtered off to yield 4-aminomethylstyrene which was used without further purification. had precipitated The solid was filtered off washed with isopropanol The mother liquor was evaporated on a rotary evaporator until no ammonia odor Isopropanol (50 mL) was then added the mixture refrigerated for several hours had precipitated was filtered off
来源 ID: ord-ea73edb555474867b190288294f09fff反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a 500 mL flask was added vinylbenzyl chloride (7.63 g, 0.050 mol), piperazine (8.61 g, 0.100 mol), and isopropanol (50 mL). The resulting solution was heated to 70° C. for 45 minutes and then cooled slowly to room temperature to form a slurry of crystalline material. The slurry was refrigerated for about three hours and then filtered. The solid piperazine hydrochloride salt was vacuum dried and then weighed (5.55 g) and discarded. The mother liquor was concentrated to about 25 mL on a rotary evaporator and ethyl acetate (50 mL) was added). The resulting mixture was refrigerated for about 10 minutes, after which a second crop of piperazine hydrochloride was filtered off and discarded. The mother liquor was then evaporated to dryness on a rotary evaporator to afford 10.135 g of crude 4-(piperazinylmethyl)styrene which was used without further purification to prepare N-(4-methylstyrene )-N'-(3-trimethylammonio-2-hydroxypropyl chloride) piperazine as follows. cooled slowly to room temperature to form a slurry of crystalline material filtered dried The mother liquor was concentrated to about 25 mL on a rotary evaporator and ethyl acetate (50 mL) was added) The resulting mixture was refrigerated for about 10 minutes after which a second crop of piperazine hydrochloride was filtered off The mother liquor was then evaporated to dryness on a rotary evaporator
来源 ID: ord-262f09c9021d43c681517d4600bdd730反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a 250 mL flask was added vinylbenzyl chloride (7.63 g, 0.050 mol), concentrated aqueous ammonia (9.8 mL), and isopropanol (40 mL). The mixture was stirred for one week, at which point a large quantity of crystalline material (ammonium chloride) had precipitated. The solid was filtered off and washed with isopropanol. The mother liquor was evaporated on a rotary evaporator until no ammonia odor could be detected. Isopropanol (50 mL) was then added, and the mixture refrigerated for several hours. Following refrigeration, ammonium chloride which had precipitated was filtered off to yield 4-aminomethylstyrene which was used without further purification. had precipitated The solid was filtered off washed with isopropanol The mother liquor was evaporated on a rotary evaporator until no ammonia odor Isopropanol (50 mL) was then added the mixture refrigerated for several hours had precipitated was filtered off
来源 ID: ord-f717c95d36a343d3ac75b5259614404f反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a 500 mL flask was added vinylbenzyl chloride (7.63 g, 0.050 mol), piperazine (8.61 g, 0.100 mol), and isopropanol (50 mL). The resulting solution was heated to 70° C. for 45 minutes and then cooled slowly to room temperature to form a slurry of crystalline material. The slurry was refrigerated for about three hours and then filtered. The solid piperazine hydrochloride salt was vacuum dried and then weighed (5.55 g) and discarded. The mother liquor was concentrated to about 25 mL on a rotary evaporator and ethyl acetate (50 mL) was added). The resulting mixture was refrigerated for about 10 minutes, after which a second crop of piperazine hydrochloride was filtered off and discarded. The mother liquor was then evaporated to dryness on a rotary evaporator to afford 10.135 g of crude 4-(piperazinylmethyl)styrene which was used without further purification to prepare N-(4-methyl-styrene)-N'-(3-trimethyl-ammonio-2-hydroxypropyl chloride) piperazine as follows. cooled slowly to room temperature to form a slurry of crystalline material filtered dried The mother liquor was concentrated to about 25 mL on a rotary evaporator and ethyl acetate (50 mL) was added) The resulting mixture was refrigerated for about 10 minutes after which a second crop of piperazine hydrochloride was filtered off The mother liquor was then evaporated to dryness on a rotary evaporator
来源 ID: ord-e5e85f3fb28e45d0861b2599e5a85f90反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Into a 2 liter volume flask equipped with a stirrer, N-methyltaurine sodium salt (161 g), deionized water (400 g) and ethylene glycol monomethyl ether (300 g) were charged. The contents were maintained at 70° C. while stirring, and a mixture of vinylbenzyl chloride (153 g), ethylene glycol monomethyl ether (100 g) and p-nitrosophenol (0.15 g) was dropwise added thereto in 1 hour, during which sodium hydroxide (each 8 g) was added thereto 6 times with intervals of 10 minutes. Thereafter, stirring was continued for 5 hours. To the reaction mixture, conc. hydrochloric acid (120 g) was added, and the resulting mixture was concentrated in a rotary evaporator to make a 1/3 volume. The concentrate was admixed with a 4 time volume of acetone and filtered. The filtrate was concentrated to a 3/10 volume and admixed with acetone. The precipitated yellow solids were collected and recrystallized from deionized water to give N-methyl-N-vinylbenzyltaurine (180 g) of the formula: Into a 2 liter volume flask equipped with a stirrer was dropwise added with intervals of 10 minutes Thereafter, stirring was continued for 5 hours the resulting mixture was concentrated in a rotary evaporator filtered The filtrate was concentrated to a 3/10 volume The precipitated yellow solids were collected recrystallized from deionized water
来源 ID: ord-9ff6caebbaaf4fde89a70b8b5b49f717反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a 100 ml flask commercial vinylbenzyl chloride (3.05 g, 0.020 mol) was mixed with hexadecyldimethylamine (5.4 g, 0.020 mol) without any additional solvent. After addition of 2,6-di-tert-butyl-4-methylphenol (100 mg, 0.45 mmol) the mixture was heated overnight at 50° C. The solid product which formed was washed several times with dry ether, dried under vacuum at room temperature, and recrystallized from acetone/ether to give 6.3 g (75%) of 4-styrylmethyl (hexadecyl)dimethylammonium chloride. 1H NMR (CDCl3 /Me4Si): 0.88 (s, 3H), 1.24 (br s, 26H ), 1.78 (s, 2H), 3.30 (s, 6H), 3.53 (s, 2H), 5.08 (s, 2H), 5.32 (d, J=10.8Hz, 1H), 5.84(d, J=18Hz, 1H), 6.7 (m, 1H), 7.51 (m, 4H). IR (KBr); 3020, 2920, 1640 cm-1. The critical micelle concentration (CMC) was 1.28× 10-2M at 25° C. determined conductometrically. The solid product which formed was washed several times with dry ether dried under vacuum at room temperature recrystallized from acetone/ether
来源 ID: ord-56bad1a205ed47fb98b2ee2a4da39f8a反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Styrene 123 g (1.18 moles), vinylbenzyl chloride 14 g (0.090 moles), divinyl benzene 30 g (0.225 moles), benzoyl peroxide 0.75 g, and 1.0 ml of mineral oil were added to 45 ml of warm water (80° C.) containing 4.5 g of soluble starch and stirred at 400 rpm at 80° C. for 24 hours. The reaction mixture was cooled and the white spherical polymer was screened through a fine mesh sieve (#100) and washed with organic solvents and water, and then dried overnight at 80° C. The polymer contained about 1.88% of chlorine. The reaction mixture was cooled washed with organic solvents and water dried overnight at 80° C
来源 ID: ord-65d4b846b7234146a81b324a689ad621反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Styrene 123 g (1.18 moles), vinylbenzyl chloride 14 g (0.090 moles), divinyl benzene 30 g (0.225 moles), benzoyl peroxide 0.75 g, and 1.0 ml of mineral oil were added to 45 ml of warm water (80° C.) containing 4.5 g of soluble starch and stirred at 400 rpm at 80° C. for 24 hours. The reaction mixture was cooled and the white spherical polymer was screened through a fine mesh sieve (#100) and washed with organic solvents and water, and then dried overnight at 80° C. The polymer contained about 1.88% of chlorine. The reaction mixture was cooled washed with organic solvents and water dried overnight at 80° C
来源 ID: ord-65d4b846b7234146a81b324a689ad621反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a 100 ml round bottom flask equipped with a stir bar, 4.0 g (26.2 mm) of vinylbenzyl chloride, and 10 ml of dimethylformamide (DMF) were added. To this solution 3.40 g (52.4 mm) of sodium azide was added and the reaction mixture was stirred at room temperature overnight, after which time 50 ml of deionized water were added to the solution. The resulting 4-vinyl benzyl azide was extracted from the reaction solution with ethyl ether. The product was confirmed by 1H NMR. To a 100 ml round bottom flask equipped with a stir bar The resulting 4-vinyl benzyl azide was extracted from the reaction solution with ethyl ether
来源 ID: ord-d6b864a90d584daf8208de4b7d8bcda2反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a 100 ml round bottom flask equipped with a stir bar, 4.0 g (26.2 mm) of vinylbenzyl chloride, and 10 ml of dimethylformamide (DMF) were added. To this solution 3.40 g (52.4 mm) of sodium azide was added and the reaction mixture was stirred at room temperature overnight, after which time 50 ml of deionized water were added to the solution. The resulting 4-vinyl benzyl azide was extracted from the reaction solution with ethyl ether. The product was confirmed by 1H NMR. To a 100 ml round bottom flask equipped with a stir bar The resulting 4-vinyl benzyl azide was extracted from the reaction solution with ethyl ether
来源 ID: ord-d6b864a90d584daf8208de4b7d8bcda2PubChem References
以下资料来自该化合物的公开数据库参考记录。
