反应详情

温度

5 °C

49.26 g of allylbicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid N-(2'-hydroxyethyl)imide (prepared according to Example 3a) and 22.26 g of triethylamine are dissolved in 160 g of toluene, and the solution is cooled under nitrogen to 5° C. With stirring, 22.91 g of methane sulfochloride are added dropwise for 1 hour, while keeping the temperature in the range from 5° to 10° C. by external cooling. The mixture is subsequently stirred for a further 18 hours at room temperature. The pH is adjusted with 1N HCl to 5 and the mixture is washed with water and dried. The product is isolated as described in Example 7. Yield: 54 g (83.0% of theory); η40°C. =2138.4 mPa.s; n25D =1.5238.

1. customfrom 5° to 10° C.
2. stirringThe mixture is subsequently stirred for a further 18 hours at room temperature
3. washthe mixture is washed with water
4. customdried
5. customThe product is isolated