反应详情

Add (diethylamino)sulfur trifluoride (3.9 mL, 29.8 mmol) to a −78° C. cooled solution of 4-(R)-hydroxypyrrolidine-N1,2-(R)-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (3.81 g, 15.54 mmol) in dichloromethane (50 mL). Stir 2 h, then remove cold bath and stir 40 h at room temperature. Cool in ice bath and add saturated sodium bicarbonate solution. Warm to room temperature, dry (magnesium sulfate), concentrate (350 mbar, 25° C.) and purify (silica gel chromatography, eluting with diethyl ether and dichloromethane) to give the title compound as an oil (4.01 g, 97%).

1. customremove cold bath
2. stirringstir 40 h at room temperature
3. temperatureCool in ice bath
4. additionadd saturated sodium bicarbonate solution
5. dry with materialdry (magnesium sulfate)
6. concentrationconcentrate (350 mbar, 25° C.)
7. custompurify
8. wash(silica gel chromatography, eluting with diethyl ether and dichloromethane)