関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetracyanoethylene | HCID 12635 | — |
| 反応物 | 1-Phenylpyrrolidine | HCID 77726 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(Pyrrolidino) tricyanovinylbenzene | HCID 54519631 | — |
反応手順
4-(pyrrolidino) tricyanovinylbenzene was prepared by mixing 1-phenylpyrrolidine (1.0 g, 6.8 mmol) with tetracyanoethylene (0.9 g, 7 mmol) in 10 mL dimethylformamide at 0° C. The reaction mixture was stirred at room temperature for three hours and at 40° C. for another ten hours. The reaction mixture was quenched with 25 mL water and the dark red colored aqueous solution was extracted with 150 mL methylene chloride and washed several times with water (150 mL). The organic layer was then separated, dried over Na2SO4 and evaporated. The crude products were purified through a silica gel column. The column was eluted with a 1:1 ratio solution of methylene chloride and hexane to yield 1.7 g of the pure product 4 (90% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05514799 |
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| 出典データセット | uspto-grants-1996_05 |
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| ORD ID | ord-40b90836aa7f4cd4a75babfddc104f60 |
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| 出典メモ | uspto-grants-1996_05 |
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