Reaktionsgleichung
[Cl:1][C:2]1[CH:15]=[CH:14][CH:13]=[CH:12][C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].[O-]CC.[Na+].[O:20]=[C:21]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH:22]=[CH2:23].Cl>C(O)C.O>[O:20]=[C:21]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH2:22][CH2:23][CH:6]([C:4](=[O:5])[C:3]1[CH:12]=[CH:13][CH:14]=[CH:15][C:2]=1[Cl:1])[C:7]([O:9][CH2:10][CH3:11])=[O:8]Komponenten
Versuchsvorschrift
To a stirred solution of 0.91 g of ethyl 2-chlorobenzoylacetate in 10 cc of ethanol was added 0.27 g of sodium ethoxide at room temperature, and the mixture was stirred at room temperature for 10 minutes. Then, 0.62 g of 3-oxo-1-decene in 10 cc of ethanol was added and the resulting mixture was stirred overnight at room temperature. Water was added to the reaction mixture, and the aqueous layer was acidified with 1N HCl and extracted three times with ethyl acetate. The combined organic layer was washed with a saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was distilled off and the crude product thus obtained was purified by a silica gel column chromatography (eluent: ethyl acetate/hexane =1/9) to obtain 0.90 g of compound I. Yield: 59.1%.
Aufarbeitung
- stirringthe resulting mixture was stirred overnight at room temperature
- extractionextracted three times with ethyl acetate
- washThe combined organic layer was washed with a saturated aqueous sodium chloride solution
- dry with materialdried over magnesium sulfate
- distillationThe solvent was distilled off
- customthe crude product thus obtained
- customwas purified by a silica gel column chromatography (eluent: ethyl acetate/hexane =1/9)
Quellen und Nachweise
- ORD-Eintrag
- ord-56de54e293c949128f37d7aafeb77437
- Quelldatensatz
- uspto-grants-1996_03
- Patentnummer
- US05500424
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