反应详情

Titanium tetrachloride (2.3 ml) was added to a mixture of 4.95 g of methyl 11-methoxy-6,11-dihydrodibenz[b,e]oxepin-3-carboxylate, 2.8 ml of ethyl cyanoacetate, 4.6 ml of diisopropylethylamine and 400 ml of benzene under ice cooling, and the mixture was stirred at room temperature for 2 days. Methanol (5 ml) was added thereto, and the mixture was diluted with ethyl acetate. The solution was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [eluent: hexane/ethyl acetate (3/1)] to give 0.72 g (11%) of the product.

1. washThe solution was washed with a saturated aqueous solution of sodium chloride
2. dry with materialdried over anhydrous magnesium sulfate
3. distillationThe solvent was distilled off under reduced pressure
4. customthe residue was purified by silica gel column chromatography [eluent: hexane/ethyl acetate (3/1)]