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Tetracyanoethylene → 2-Cyano-3-(4-dibutylamino-2-methoxyphenyl)-2-butenedinitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetracyanoethylene | HCID 12635 | — |
| 反応物 | N,N-Dibutyl-3-methoxybenzenamine | HCID 4068285 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Cyano-3-(4-dibutylamino-2-methoxyphenyl)-2-butenedinitrile | HCID 86193774 | 77.2% |
反応手順
In 8 ml of N,N-dimethylformamide, 0.5 g (3.9 mmol) of tetracyanoethylene was dissolved. With stirring under ice cooling, 0.8 g (3.4 mmol) of dibutyl(3-methoxyphenyl)amine was dissolved in 2 ml of N,N-dimethylformamide and added dropwise. The mixture was stirred for 35 minutes. After the ice bath was removed, the mixture was further stirred for 2 hours. After the reaction mixture was poured into 100 ml of water, extraction with chloroform, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residue was purified by silica gel column chromatography and washed with hexane to give 0.88 g of a black crystal having a mp of 86° C. (yield: 77.2%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846955B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-392e4ffe9a4b4b3cbb42e9ad5c532ef5 |
| 出典メモ | uspto-grants-2014_09 |