反应详情

温度

-100 °C

A solution of 4.81 8 (0.01747 mol) of 2-[1-(1H-inden-3-yl)-1-methyl-4-pentenyl]pyridine in 60 ml of tetrahydrofuran was cooled to −100° C. 11.5 ml of a 15% strength n-butyllithium solution in hexane (0.01834 mol) were slowly added dropwise. After the addition was complete, the reaction mixture was stirred at −100° C. for a further 1 hour. The mixture was subsequently allowed to warm to room temperature. After stirring for a further 2 hour, the solution was cooled to 60° C. and 7.07 g (0.0189 mol) of chromium trichloride tris(tetrahydrofuran) were added while stirring. The mixture was allowed to warm slowly to room temperature and was subsequently stirred at room temperature for a further 10 hours. The solid which had precipitated was filtered off, washed with diethyl ether and dried under reduced pressure. Recrystallization from a mixture of dichloromethane and diethyle ether gave 2.5 g of (3-(2-pyridyl-1-methyl-4-pentenyl)indenyl)chromium dichloride (36%).

1. additionAfter the addition
2. temperatureto warm to room temperature
3. stirringAfter stirring for a further 2 hour
4. temperaturethe solution was cooled to 60° C.
5. stirringwhile stirring
6. temperatureto warm slowly to room temperature
7. stirringwas subsequently stirred at room temperature for a further 10 hours
8. customThe solid which had precipitated
9. filtrationwas filtered off
10. washwashed with diethyl ether
11. customdried under reduced pressure
12. customRecrystallization
13. additionfrom a mixture of dichloromethane