反应详情

温度

-78 °C

n-Butyllithium (50 ml of 1.53 M heptane solution) was introduced into a previously dried and nitrogen purged 100 ml Pyrex-glass pressure tube equipped with a perforated crown cap over a self-sealing rubber gasket. After adjusting the temprature of this solution to -78° C., 20 ml of tetrahydrofuran and 8 ml of 1,3,5-cycloheptatriene (0.077 moles) were added. The solution turned red in color almost immediately after addition of the 1,3,5-cycloheptatriene. This reaction mixture was maintained at -78° C. for 15 minutes. The temperature was adjusted to 0° C. and the solution maintained at this temperature for one hour. During this period the solution became very dark in color. Dilution of 38 ml of this n-butylcycloheptadienyllithium solution with 279 ml of toluene gave a red-violet solution having a molarity of 0.1255 as determined by disulfide titration. This titration method is described in C. A. Uraneck, J. E. Burleigh, and J. W. Cleary, Analytical Chemistry 40, 327 (1968).

1. customa previously dried
2. customnitrogen purged 100 ml Pyrex-glass pressure tube
3. customequipped with a perforated crown
4. customcap over a self-sealing rubber gasket
5. customto -78° C.
6. customwas adjusted to 0° C.
7. temperaturethe solution maintained at this temperature for one hour
8. waitDuring this period the solution became very dark in color