反应详情

温度

20 °C

Tropine (50 g) and diisopropylethylamine (48.05 g) in dichloromethane (0.5 L) were cooled to −10° C. Methane sulphonyl chloride (44.7 g) in dichloromethane (0.125 L) was added over 0.75 h at <−5° C. After 0.5 h a solution of potassium carbonate (75 g) in water (0.2 L) was added and the mixture warmed to 20° C. The phases were separated and the dichloromethane solution concentrated by distillation under reduced pressure at <20° C. to leave a residue whereby the dichloromethane content was 51% w/w. Heptane (0.05 L) was added and the solution cooled to 0° C. to crystallize the title compound. Further heptane (0.45 L) was added and the mixture kept under vacuum (350 mbar) at 20-25° C. until the dichloromethane content was 8% w/w. The mixture was cooled to 0° C. and stirred for 1 h. The product was isolated by filtration, washed and dried at <30° C. to give the title compound (68.5 g, 88.1%).

1. customThe phases were separated
2. concentrationthe dichloromethane solution concentrated by distillation under reduced pressure at <20° C.
3. customto leave a residue whereby the dichloromethane content
4. temperaturethe solution cooled to 0° C.
5. customto crystallize the title compound
6. additionFurther heptane (0.45 L) was added
7. customkept under vacuum (350 mbar) at 20-25° C. until the dichloromethane content
8. temperatureThe mixture was cooled to 0° C.
9. customThe product was isolated by filtration
10. washwashed
11. customdried at <30° C.