関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | 1-(6-Methylpyridin-3-yl)butane-1,3-dione | HCID 20212814 | — |
| 生成物 | Ethyl 6-methylnicotinate | HCID 281994 | — |
反応手順
The 6-methylnicotinoyl-acetone which is mentioned as the starting substance in Example 6, can be obtained in a known manner from α-picoline-5-carboxylic acid ethyl ester and acetone, or from 5-acetyl-α-picoline (prepared in accordance with Angew. Ch. 67, page 398) and ethyl acetate: 270 g of 5-acetyl-α-picoline, 5 1 of anhydrous toluene, 387 g. of ethyl acetate and 537 g of potassium tert.-butylate are stirred at 40° for 20 hours and the mixture is subsequently decomposed by means of a mixture of 3 1 of ice water and 288 ml of acetic acid. 283.5 g of 6-methylnicotinoyl-acetone, boiling point 108°-117° /0.2 mm Hg, which rapidly crystallises and, after recrystallisation from ligroin, melts at 57°-58°, is obtained in the usual manner from the toluene solution.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04088764 |
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| 出典データセット | uspto-grants-1978_05 |
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| ORD ID | ord-540a9718c8b849a59be9cb99481e71a2 |
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| 出典メモ | uspto-grants-1978_05 |
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