反应详情

Triethylamine (18.5 ml, 0.134 moles) was dropwise added to a suspension of (5-methoxy-3-oxo-1,3-dihydro-isobenzofuran-1-yl)triphenyl phosphonium bromide (74 g. 0.134 moles) obtained as described in example 10, and 3,5-dichloro-pyridin-4-carbaldehyde (23.6 g, 0.134 moles) in CH2Cl2 (500 ml) under N2 by controlling the temperature with a water-bath. The mixture was kept under stirring overnight, then cooled and treated with 5% HCl. The phases were separated and the acid one was re-extracted with CH2Cl2, washed with water/NaCl, decoloured with charcoal, dried and concentrated under 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. customobtained
2. temperaturecooled
3. customThe phases were separated
4. extractionthe acid one was re-extracted with CH2Cl2
5. washwashed with water/NaCl
6. customdried
7. concentrationconcentrated under high vacuum
8. customThere were obtained 85.4 g of a crude which
9. customA sample of the crude was purified by flash chromatography (eluent:hexane/ethyl acetate 1:1)