Reaktionsgleichung
[C:1](OC)(=O)[CH2:2][C:3]([O:5]C)=O.[CH3:10][O-].[Na+].[C:13]1([CH3:19])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>>[CH3:19][C:13]1[CH:18]=[CH:17][C:16]([CH:1]=[CH:2][C:3](=[O:5])[CH3:10])=[CH:15][CH:14]=1Komponenten
Versuchsvorschrift
132 g of dimethyl malonate are introduced into 1 liter of toluene and 180 g of 30% strength sodium methylate solution are added at room temperature. A crystal slurry results, to which 160 g of p-methylbenzalacetone are added dropwise, with vigorous stirring. In the course of 3 hours, the reaction mixture is heated, with methanol distilling off azeotropically, until the temperature at which the vapors pass over has reached 110° C. 106 g of butyryl chloride are then added at 80°-90° C. and stirring is continued briefly. 5 g of 4-N,N-dimethylaminopyridine are added, the mixture is stirred for 3-4 hours at 100° C. and the solvent is then evaporated. A solution of 120 g of sodium hydroxide in 1.5 liters of water is added to the residue and the mixture is stirred for 2 hours at 80° C. It is then acidified with 270 ml of concentrated hydrochloric acid at 60° C., and when the mixture has cooled to room temperature the precipitate is filtered off with suction and washed neutral with water. After it has been dried, 239 g (88%) of 2-butyryl-5-(p-toluyl)-cyclohexane-1,3-dione, of melting point 76°-78° C., are obtained.
Aufarbeitung
- additionare added at room temperature
Quellen und Nachweise
- ORD-Eintrag
- ord-ecd7981a6eeb4d8382517df73fb966d0
- Quelldatensatz
- uspto-grants-1992_06
- Patentnummer
- US05118856
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