Reaktionsgleichung
[CH3:1][C:2]1[CH:13]=[CH:12][C:5]([C:6](CC(=O)C)=[O:7])=[CH:4][N:3]=1.[CH3:14][C:15](C)=[O:16]>>[CH2:15]([O:16][C:6]([C:5]1[CH:12]=[CH:13][C:2]([CH3:1])=[N:3][CH:4]=1)=[O:7])[CH3:14]Komponenten
Versuchsvorschrift
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.
Quellen und Nachweise
- ORD-Eintrag
- ord-540a9718c8b849a59be9cb99481e71a2
- Quelldatensatz
- uspto-grants-1978_05
- Patentnummer
- US04088764
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