反应详情

To a stirred, ice-cooled solution of 2,5-diphenyl-3-hydroxythiophene (0.12 g, 0.5 mmol) in dried pyridine (5.0 ml) under a nitrogen atmosphere was added 3-carbomethoxypropionyl chloride (0.1 g, 0.66 mmol) over ca. 20 seconds. The mixture was allowed to stir cold for 15 minutes and then at ambient temperatures for 4 hours. The mixture was added in portions to a stirred mixture of ether, ice, water, and 2N hydrochloric acid (40 ml), the ether layer washed 2 times with water, dried over sodium sulfate, filtered and concentrated to 0.18 g of oily (I). M.S.: M+ =366; NMR: consistent. ##STR26##

1. waitat ambient temperatures for 4 hours
2. washthe ether layer washed 2 times with water
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated to 0.18 g of oily (I)