反应详情

温度

70 °C

To a mixture of 7.9 g of cesium carbonate and 15 ml of dimethyl sulfoxide was added 4.2 ml of acetic acid. After foaming ceased, a mixture of 14.4 g of 2-benzyl-3-iodo-6-[(3S,4S)-3-(3-nitrobenzenesulfonyl)oxy-4-methoxypyrrolidin-1-yl]pyridine and 35 ml of dimethyl sulfoxide was added and the resultant mixture was heated under stirring under nitrogen atmosphere in an oil bath at 70° C. for 6 hours. After the reaction mixture was cooled, it was extracted with ethyl acetate-water. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (10–15% ethyl acetate/hexane), to give 7.5 g of the title compound.

1. additionwas added
2. temperatureAfter the reaction mixture was cooled
3. extractionit was extracted with ethyl acetate-water
4. washThe organic layer was washed with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography (10–15% ethyl acetate/hexane)