反应详情

4.2 ml of acetic acid was added to a mixture of 7.9 g of cesium carbonate and 15 ml of dimethyl sulfoxide. After foaming stopped, a mixture of 14.4 g of 2-benzyl-3-iodo-6-[(3S,4S)-3-(3-nitrobenzenesulfonyl)oxy-4-methoxypyrrolidine-1-yl]pyridine and 35 ml of dimethyl sulfoxide was added thereto, followed by heating under stirring for 6 hours in an oil bath kept at 70° C. in a nitrogen atmosphere. The reaction solution was cooled and then subjected to extraction with ethyl acetate-water. The organic phase was washed with water and brine brine, dried over anhydrous magnesium sulfate and then concentrated. The residue was subjected to silica gel column chromatography using 10-15% ethyl acetate/hexane, to give 7.5 g of the target compound.

1. additionwas added
2. temperatureby heating
3. customkept at 70° C. in a nitrogen atmosphere
4. temperatureThe reaction solution was cooled
5. extractionsubjected to extraction with ethyl acetate-water
6. washThe organic phase was washed with water and brine brine
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated