Zirconocene dichioride → Bis(5-methylcyclopenta-1,3-diene);zirconium(2+)

HRID 1603978ノート

反応式

HRID 1603978 の反応式
C[Li].[Cl-].[Cl-].[CH-:5]1[CH:9]=[CH:8][CH:7]=[CH:6]1.[CH-:10]1[CH:14]=[CH:13][CH:12]=[CH:11]1.[Zr+2:15]>C(OCC)C>[CH3:10][C-:5]1[CH:9]=[CH:8][CH:7]=[CH:6]1.[C-:10]1([CH3:5])[CH:14]=[CH:13][CH:12]=[CH:11]1.[Zr+2:15]

参加物

4

反応物 2

HCID 131716798Zirconocene dichiorideHCID 178418348HCID 178418348、化合物

生成物 1

HCID 129652697Bis(5-methylcyclopenta-1,3-diene);zirconium(2+)収率 211%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Following the literature procedure [b], 3.30 ml (5.33 mmol, 1.60 M) of an ethereal solution of methyllithium are slowly added dropwise at -78° C. to a suspension of 1.03 g (2.66 mmol) of zirconocene dichloride (Example 10) in 50 ml of diethyl ether. The mixture is allowed to warm slowly to room temperature in a cold bath and is then stirred at room temperature for a further 5 hours. The solvent is removed in vacuo, and the colorless residue is extracted with 3×50 ml of pentane. The combined pentane solutions are evaporated and kept at -25° C. to crystallize. Removal of the solvent and drying in an oil-pump vacuum gives 700 mg (76%) of dimethylzirconocene as a colorless, crystalline powder.

後処理

  1. customThe solvent is removed in vacuo
  2. extractionthe colorless residue is extracted with 3×50 ml of pentane
  3. customThe combined pentane solutions are evaporated
  4. customkept at -25° C.
  5. customto crystallize
  6. customRemoval of the solvent
  7. customdrying in an oil-pump vacuum

出典と根拠

ORDレコード
ord-c7984ef718134880bfd2b9e5a247882f
出典データセット
uspto-grants-1999_11
特許番号
US05990254

反応ノート

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