2-(2,2-dimethylpropanoyl)propanedinitrile

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

実験手順: Phosphorous pentachloride (86 g) was added slowly to a stirred suspension of the above pivaloylmalononitrile intermediate (a) (57 g) in methylene chloride (500 ml) and was allowed to stir at room temperature for 16 hours. Sulfur dioxide was passed through the solution for 20 minutes and the solvent was removed on a rotary evaporator. The residue was poured onto ice and filtered. The product was used without further purification. the solvent was removed on a rotary evaporator The residue was poured onto ice filtered The product was used without further purification

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

実験手順: Pivaloyl chloride (60 g) and malononitrile (33g) were dissolved in methylene chloride (500 ml) and were placed in a flask equipped with a stirrer and a dropping funnel. Triethylamine (100 g) was added slowly with cooling over a period of 45 minutes. The triethylamine hydrochloride was removed and the filtrate was concentrated to about half volume. The solution was poured onto ice, acidified strongly with concentrated hydrochloric acid and the resulting product was filtered off and air dried. were placed in a flask equipped with a stirrer and a dropping funnel with cooling over a period of 45 minutes The triethylamine hydrochloride was removed the filtrate was concentrated to about half volume The solution was poured onto ice the resulting product was filtered off air dried

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

実験手順: Phosphorous pentachloride (86 g) was added slowly to a stirred suspension of the above pivaloylmalononitrile intermediate (a) (57 g) in methylene chloride (500 ml) and was allowed to stir at room temperature for 16 hours. Sulfur dioxide was passed through the solution for 20 minutes and the solvent was removed on a rotary evaporator. The residue was poured onto ice and filtered. The product was used without further purification. the solvent was removed on a rotary evaporator The residue was poured onto ice filtered The product was used without further purification

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

実験手順: Pivaloyl chloride (60 g) and malononitrile (33 g) were dissolved in methylene chloride (500 ml) and were placed in a flask equipped with a stirrer and a dropping funnel. Triethylamine (100 g) was added slowly with cooling over a period of 45 minutes. The triethylamine hydrochloride was removed and the filtrate was concentrated to about half volume. The solution was poured onto ice, acidified strongly with concentrated hydrochloric acid and the resulting product was filtered off and air dried. were placed in a flask equipped with a stirrer and a dropping funnel with cooling over a period of 45 minutes The triethylamine hydrochloride was removed the filtrate was concentrated to about half volume The solution was poured onto ice the resulting product was filtered off air dried

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

実験手順: Phosphorous pentachloride (86 g) was added slowly to a stirred suspension of the above pivaloylmalononitrile intermediate (a) (57 g) in methylene chloride (500 ml) and was allowed to stir at room temperature for 16 hours. Sulfur dioxide was passed through the solution for 20 minutes and the solvent was removed on a rotary evaporator. The residue was poured onto ice and filtered. The product was used without further purification. the solvent was removed on a rotary evaporator The residue was poured onto ice filtered The product was used without further purification

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

実験手順: Pivaloyl chloride (60 g) and malononitrile (33g) were dissolved in methylene chloride (500 ml) and were placed in a flask equipped with a stirrer and a dropping funnel. Triethylamine (100 g) was added slowly with cooling over a period of 45 minutes. The triethylamine hydrochloride was removed and the filtrate was concentrated to about half volume. The solution was poured onto ice, acidified strongly with concentrated hydrochloric acid and the resulting product was filtered off and air dried. were placed in a flask equipped with a stirrer and a dropping funnel with cooling over a period of 45 minutes The triethylamine hydrochloride was removed the filtrate was concentrated to about half volume The solution was poured onto ice the resulting product was filtered off air dried