反応 #76113

反応方程式

chromium(III)chloride

potassium hydride

1-(8-quinolyl)indene

→

1-(8-quinolyl)indenylchromium(III) dichloride

収率 50.0%

溶媒

THF

THF

反応条件

後処理

1. 1
   workup.ADDITIONwhen the addition
2. 2
   workup.STIRRINGthe mixture was stirred for a further 16 hours
3. 3
   その他The solvent was removed
4. 4
   抽出the resultant solid was extracted with hot toluene
5. 5
   workup.DISTILLATIONAfter the solvent had been distilled off from the combined extracts
6. 6
   その他the product was obtained as a green powder, which
7. 7
   洗浄was washed a number of times with hexane
8. 8
   その他dried under a high vacuum

実験手順

0.05 g of potassium hydride (1.23 mmol) was suspended in 20 ml of THF, and 0.3 g of 1-(8-quinolyl)indene (1.23 mmol) was slowly added. The resultant violet suspension was stirred at room temperature for three hours and then added dropwise to a mixture of 0.46 g of chromium(III)chloride 3THF (1.23 mmol) in 50 ml of THF and, when the addition was complete, the mixture was stirred for a further 16 hours. The solvent was removed under reduced presssure, and the resultant solid was extracted with hot toluene. After the solvent had been distilled off from the combined extracts, the product was obtained as a green powder, which was washed a number of times with hexane and dried under a high vacuum, giving 0.22 g of 1-(8-quinolyl)indenylchromium(III) dichloride (50%).

出典