chloroethene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Degassed anhydrous tetrahydrofuran (500 mL) was added to 5.86 g (4.32 mmol) solid tetrakis(triphenylphosphine) palladium(O) and copper (I) iodide (5.17 g, 27.1 mmol) stirring under argon. A solution of the vinyl chloride (compound M of step (a) 45.38 g, 226.1 mmol) in 100 mL of dry tetrahydrofuran was added via cannula followed immediately by the addition of 45 mL (455 mmol) neat butylamine. The flask was wrapped in aluminum foil to exclude light and then 41.6 mL (294 mmol) of trimethylsilyl acetylene was added via syringe over 4 min. After about 10 min the reaction became very warm and was cooled in an ice water bath for 3 min. The cooling bath was then removed and the reaction allowed to stir for 4h at ambient temperature. Air was bubbled through the reaction for 15 min and then the reaction was filtered by suction through a glass frit using pentane then ether washes for transfer. The reaction was diluted with ether and washed with five 500 ml portions of water. The aqueous washes were reextracted with a small amount of diethyl ether and the combined organic extracts were dried over anhydrous Na2SO4, filtered, and concentrated on a rotary evaporator. Flash chromatography over SiO2 using 2.5% to 4% ethyl acetate/hexane as eluent provided 52.86 g (89%) of liquid as the desired product: Degassed anhydrous tetrahydrofuran (500 mL) After about 10 min the reaction became very warm was cooled in an ice water bath for 3 min The cooling bath was then removed to stir for 4h at ambient temperature Air was bubbled through the reaction for 15 min the reaction was filtered by suction through a glass frit The reaction was diluted with ether washed with five 500 ml portions of water the combined organic extracts were dried over anhydrous Na2SO4 filtered concentrated on a rotary evaporator

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Degassed anhydrous tetrahydrofuran (500 mL) was added to 5.86 g (4.32 mmol) solid tetrakis(triphenylphosphine) palladium(O) and copper (I) iodide (5.17 g, 27.1 mmol) stirring under argon. A solution of the vinyl chloride (compound M of step (a) 45.38 g, 226.1 mmol) in 100 mL of dry tetrahydrofuran was added via cannula followed immediately by the addition of 45 mL (455 mmol) neat butylamine. The flask was wrapped in aluminum foil to exclude light and then 41.6 mL (294 mmol) of trimethylsilyl acetylene was added via syringe over 4 min. After about 10 min the reaction became very warm and was cooled in an ice water bath for 3 min. The cooling bath was then removed and the reaction allowed to stir for 4h at ambient temperature. Air was bubbled through the reaction for 15 min and then the reaction was filtered by suction through a glass frit using pentane then ether washes for transfer. The reaction was diluted with ether and washed with five 500 ml portions of water. The aqueous washes were reextracted with a small amount of diethyl ether and the combined organic extracts were dried over anhydrous Na2SO4, filtered, and concentrated on a rotary evaporator. Flash chromatography over SiO2 using 2.5% to 4% ethyl acetate/hexane as eluent provided 52.86 g (89%) of liquid as the desired product: Degassed anhydrous tetrahydrofuran (500 mL) After about 10 min the reaction became very warm was cooled in an ice water bath for 3 min The cooling bath was then removed to stir for 4h at ambient temperature Air was bubbled through the reaction for 15 min the reaction was filtered by suction through a glass frit The reaction was diluted with ether washed with five 500 ml portions of water the combined organic extracts were dried over anhydrous Na2SO4 filtered concentrated on a rotary evaporator

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An autoclave equipped with a stirrer was charged with methanol, vinyl chloride, vinyl acetate, di(2-ethylhexyl) peroxydicarbonate and partially saponified polyvinyl alcohol, and the temperature was elevated to 60° C. with stirring under an atmosphere of nitrogen gas to initiate the reaction, followed by further continuous injection of vinyl chloride to conduct the copolymerization reaction. After release of the residual pressure of the autoclave and cooling, a copolymer slurry was taken out and filtered, followed by washing with methanol three times and further with deionized water twice. Then, the resulting product was filtered and dried to obtain a vinyl chloride-vinyl acetate copolymer powder. This copolymer, methanol, N,N-dimethylethanolamine and sodium hydroxide were added to a reactor equipped with a cooling pipe, and were allowed to react at 40° C. Then, the reaction product was cooled, and acetic acid was added thereto to neutralize unreacted sodium hydroxide. The resulting product was washed with methanol three times and further with deionized water twice, followed by filtering and drying to obtain a vinyl chloride-vinyl acetate-vinyl alcohol-N,N-dimethylethanolamine-modified vinyl unit copolymer powder. An autoclave equipped with a stirrer was elevated to 60° C. the reaction the copolymerization reaction After release of the residual pressure of the autoclave and cooling filtered by washing with methanol three times and further with deionized water twice Then, the resulting product was filtered dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An autoclave equipped with a stirrer was charged with methanol, vinyl chloride, vinyl acetate, di(2-ethylhexyl) peroxydicarbonate and partially saponified polyvinyl alcohol, and the temperature was elevated to 60° C. with stirring under an atmosphere of nitrogen gas to initiate the reaction, followed by further continuous injection of vinyl chloride to conduct the copolymerization reaction. After release of the residual pressure of the autoclave and cooling, a copolymer slurry was taken out and filtered, followed by washing with methanol three times and further with deionized water twice. Then, the resulting product was filtered and dried to obtain a vinyl chloride-vinyl acetate copolymer powder. This copolymer, methanol and sodium hydroxide were added to a reactor equipped with a cooling pipe, and were allowed to react at 40° C. Then, the eaction product was cooled, and acetic acid was added thereto to neutralize unreacted sodium hydroxide. The resulting product was washed with methanol three times and further with deionized water twice, followed by filtering and drying to obtain a vinyl chloride-vinyl acetate-vinyl alcohol copolymer powder. An autoclave equipped with a stirrer was elevated to 60° C. the reaction the copolymerization reaction After release of the residual pressure of the autoclave and cooling filtered by washing with methanol three times and further with deionized water twice Then, the resulting product was filtered dried