関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Diacetylpyridine | HCID 70790 | — |
| 反応物 | 2-Chloro-4,6-dimethylaniline | HCID 113033 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,6-Bis[1-(2-chloro-4,6-dimethylphenylimino)ethyl]pyridine | HCID 58097740 | 74.7% |
反応手順
To a solution of 2,6-diacetylpyridine (35 g, 0.21 mol) in THF (1.21) was added 2-chloro-4,6-dimethylaniline (76.7 g, 2.3 eq) and Sicapent (45 g). The reaction mixture was refluxed overnight. Then additional 2-chloro-4,6-dimethylaniline (25 g, 0.7 eq) and Sicapent (25 g) were added and once again refluxed overnight. The suspension was cooled to 22° C., filtered and washed with two times THF (75 ml). The mother liquor was concentrated (90%) and methanol was added to precipitate the product, which was washed two times with methanol (50 ml) and dried under high vacuum. 68.8 g of a yellow powder was isolated (y=73.1%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08759460B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-afeb893ab894431d89fb4142e79dd804 |
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| 出典メモ | uspto-grants-2014_06 |
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