関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Acetylpyridine | HCID 14286 | — |
| 反応物 | 2,3,5,6-Tetramethyl-1,4-phenylenediamine | HCID 76548 | — |
| 触媒 | Formic Acid | HCID 284 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,3,5,6-tetramethyl-N-(1-pyridin-2-ylethylidene)-benzene-1,4-diamine | HCID 86083572 | 445.9% |
反応手順
To a mixture of 2-acetylpyridine (0.30 ml, 0.26 mmol) and 2,3,5,6-tetramethyl-benzene-1,4-diamine (0.60 g, 0.37 mmol, 1.4 eq.) in toluene (2 ml) was added 2 drops of formic acid. The suspension was heated for three days at 50° C. The dark reddish suspension was cooled, filtered and the residue washed with cold toluene. The filtrate was evaporated, dissolved in chloroform (2 ml) and cooled to −78° C. for 0.5 hours before being filtered. Hexane was added to the filtrate and all volatiles were removed under reduced pressure to give 2,3,5,6-tetramethyl-N-(1-pyridin-2-ylethylidene)-benzene-1,4-diamine as a brown solid (0.31 g, 45%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741240B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-8ce7c26fc9964d679eb3ceefa671fdef |
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| 出典メモ | uspto-grants-2010_06 |
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