Potassium hydride → HCID 178478635, compound

HRID 47835Notes

Reaction equation

HRID 47835 reaction equation
[H-].[K+].[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14]2)[CH:6]=[CH:5][CH:4]=1.[Cl-:22].[Cr+3:23].[Cl-].[Cl-]>C1COCC1>[Cl-:22].[Cl-:22].[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[C:14]2[Cr+2:23])[CH:6]=[CH:5][CH:4]=1

Participants

5

Reactant 3

HCID 82127Potassium hydrideHCID 6452300Chromium(3+) trichlorideHCID 219779971-(8-Quinolyl)indene

Product 1

HCID 178478635HCID 178478635, compoundYield 50%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

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%).

Workup

  1. additionwhen the addition
  2. stirringthe mixture was stirred for a further 16 hours
  3. customThe solvent was removed
  4. extractionthe resultant solid was extracted with hot toluene
  5. distillationAfter the solvent had been distilled off from the combined extracts
  6. customthe product was obtained as a green powder, which
  7. washwas washed a number of times with hexane
  8. customdried under a high vacuum

Sources & evidence

ORD record
ord-105ab193db6e4b0598a3e3b46ccd1081
Source dataset
uspto-grants-2004_03
Patent number
US06699948B2

Reaction notes

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