反应 #1365723

ord-cac2c426618943b8a3cfe6d4d1c9914d

反应方程式

Cc1ccc(C)c2c1C=CC2
4,7-dimethylindene
[Li][CH2]CCC
n-butyl-lithium
[Li][CH]1C=Cc2c(C)ccc(C)c21
4,7-dimethylindenyllithium

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他whole to again reach room temperature

实验过程

38.2 g (265 mmol) of 4,7-dimethylindene were dissolved in 350 ml of tetrahydrofuran and the temperature of the solution was raised to 0° C. Thereafter, 165 ml of n-butyl-lithium (1.6M in hexane, 264 mmol) were added dropwise over 2.5 hours. After having allowed the whole to again reach room temperature and whilst stirring for 4 hours, a purple-red solution of 4,7-dimethylindenyllithium was obtained. This solution was cooled to −70° C. and treated, dropwise for 35 minutes, with 25.3 g of 1,2-dibromethane (135 mmol) in 15 ml of tetrahydrofuran. After the temperature was raised again to room temperature, a light yellow solution was obtained to which water was added. The organic phase was collected and dried on Na2SO4. The solvent was then evaporated under vacuum and 20 g of product (yield 48%) were obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06444604B1uspto-grants-2002_09