[H-].[Na+].[N:3]1([CH2:8]P(=O)(OCC)OCC)[CH:7]=[N:6][CH:5]=[N:4]1.[CH3:17][C:18]([CH3:31])([C:20](=O)[CH2:21][O:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=1)[CH3:19].C1OCCOCCOCCOCCOC1>C(COC)OC>[N:3]1([CH:8]=[C:20]([CH2:21][O:22][C:23]2[CH:24]=[CH:25][C:26]([Cl:29])=[CH:27][CH:28]=2)[C:18]([CH3:31])([CH3:17])[CH3:19])[CH:7]=[N:6][CH:5]=[N:4]1
15 g of sodium hydride in the form of a 55% dispersion in oil are added under nitrogen to 150 ml of 1,2-dimethoxyethane. Then a solution of 69 g (0.315 mole) of diethyl (1H-1,2,4-triazol-1-yl)methylphosphonate, 68 g (0.3 mole) of 2,2-dimethyl-4-(4-chlorophenoxy)butan-3-one and a trace of 15-crown-5 in 500 ml of dimethoxyethane are added dropwise. The reaction mixture is stirred for about 10 hours and, after the dropwise addition of ice/water, extracted with methylene chloride. The combined extracts are washed with water, dried over sodium sulfate, filtered and concentrated. The oily residue is purified by column chromatography over silica gel with a 4:2:2:2 mixture of toluene/cyclohexane/diethyl ether/dichloromethane as eluant, affording the product in the form of a yellow oil.
Wird geladen…
