反应详情

A suspension under N2 of (5-methoxy-3-oxo-1,3-dihydro-isobenzofuran-1-yl)-triphenyl-phosphonium bromide (74 g, 0.134 mole), prepared as described in example 36, and 3,5-dichloro-pyridin-4-carbaldehyde (23.6 g, 0.134 mole) in CH2Cl2 (500 ml) was dropwise added with triethylamine (18.5 ml, 0.134 mole), adjusting the temperature with a water bath. The mixture was stirred overnight, then cooled and treated with 5% HCl. The phases were separated and the acidic one was extracted with CH2Cl2, washed with H2O/NaCl, discoloured with charcoal, anhydrified and concentrated at high vacuum. There were obtained 85.4 g of a crude which was used as such in the subsequent step. A sample of the crude was purified by flash chromatography (eluent: hexane/ethyl acetate 1:1).

1. temperaturecooled
2. customThe phases were separated
3. extractionthe acidic one was extracted with CH2Cl2
4. washwashed with H2O/NaCl
5. concentrationconcentrated at high vacuum
6. customThere were obtained 85.4 g of a crude which
7. customA sample of the crude was purified by flash chromatography (eluent: hexane/ethyl acetate 1:1)