반응 #76113

ord-105ab193db6e4b0598a3e3b46ccd1081

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06699948B2uspto-grants-2004_03