반응 #580586

반응 방정식

chromium trichloride bis(tetrahydrofuran)

n-butyllithium

hexane

pyridine

→

(3-(2-pyridyl-1-methylethyl)indenyl)chromium dichloride

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   온도to warm to room temperature
3. 3
   workup.STIRRINGAfter stirring for a further 1 hour
4. 4
   온도the solution was cooled to −60° C.
5. 5
   workup.STIRRINGwhile stirring
6. 6
   온도to warm slowly to room temperature
7. 7
   workup.STIRRINGwas subsequently stirred for a further 10 hours at room temperature
8. 8
   온도The reaction mixture was then refluxed for 20 minutes
9. 9
   온도subsequently cooled to room temperature
10. 10
    기타The solid which had precipitated
11. 11
    여과was filtered off
12. 12
    세척washed with diethyl ether
13. 13
    기타dried under reduced pressure

실험 절차

A solution of 0.54 g (0.0023 mol) of [2-1H-inden-3-yl)-1-methylethyl]pyridine in 20 ml of tetrahydrofuran was cooled to −100° C. 1.72 ml of a 15% strength n-butyllithium solution in hexane (0.0027 mol) were slowly added dropwise. After the addition was complete, the reaction mixture was stirred at −100° C. for a further 30 minutes. The mixture was subsequently allowed to warm to room temperature. After stirring for a further 1 hour, the solution was cooled to −60° C. and 1.1 g (0.0029 mol) of chromium trichloride bis(tetrahydrofuran) were added while stirring. The mixture was allowed to warm slowly to room temperature and was subsequently stirred for a further 10 hours at room temperature. The reaction mixture was then refluxed for 20 minutes and subsequently cooled to room temperature. The solid which had precipitated was filtered off, washed with diethyl ether and dried under reduced pressure. This gave 0.3 g of (3-(2-pyridyl-1-methylethyl)indenyl)chromium dichloride (37%).

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