反应详情

温度

50 °C

To an ice-cold solution of 170 g (626.5 mmol) of (2R, 4S)-2-hydroxymethyl-4-hydroxy-1-(4-toluenesulfonyl)-pyrrolidine in 0.5 l of pyridine was added 250 g (1.32 mol) of p-toluenesulfonyl chloride in one portion and the reaction was warmed to 50° C. After 6 hours the mixture was cooled with an ice bath and 3 l of 10% aqueous hydrogen chloride solution was carefully added. A white precipitate formed which was isolated via filtration and then taken in 1 l of ethanol and heated to reflux for 30 minutes. The mixture was then cooled and the solids were filtered and dried under reduced pressure to give 195 g of product in 70% yield. M.P.=145°-146° C.

1. temperatureAfter 6 hours the mixture was cooled with an ice bath
2. customA white precipitate formed which
3. customwas isolated via filtration
4. temperatureheated
5. temperatureto reflux for 30 minutes
6. temperatureThe mixture was then cooled
7. filtrationthe solids were filtered
8. customdried under reduced pressure