反应详情

温度

50 °C

A solution of 1-bromo-2-pentyne (0.51 g, 3.44 mmol) in chloroform (2 ml) is treated with polymer supported TEA resin. After a few minutes this solution is added to a solution of hydroxy-di-thiophen-2-yl-acetic acid (R)-(1-aza-bicyclo-[2.2.2]oct-3-yl) ester (Example 70(ii)) (1.0 g, 2.87 mmol) in chloroform (2 ml). The resulting mixture is heated to 50° C. for 18 h and the mixture allowed to cool to room temperature. A white solid is isolated by filtration, washed with chloroform and dried. Recrystallisation from chloroform-acetonitrile, washing the resultant solid with cold acetonitrile, and drying under vacuum gives (R)-3-(2-Hydroxy-2,2-di-thiophen-2-yl-acetoxy)-1-pent-2-ynyl-1-azonia-bicyclo[2.2.2]octane bromide.

1. temperatureto cool to room temperature
2. customA white solid is isolated by filtration
3. washwashed with chloroform
4. customdried
5. customRecrystallisation from chloroform-acetonitrile
6. washwashing the resultant solid with cold acetonitrile
7. customdrying under vacuum