Toluene → Cyclopenta-1,3-diene;hafnium(4+);dichloride

HRID 1603977

반응식

HRID 1603977 반응식
[Cl-:1].[Cl-].[Cl-].[Cl-].[Hf+4:5].[Li][Li].[C:8]1([CH3:14])[CH:13]=[CH:12][CH:11]=CC=1>>[CH2:12]1[C-:11]=[CH:14][CH:8]=[CH:13]1.[CH2:12]1[C-:11]=[CH:14][CH:8]=[CH:13]1.[Cl-:1].[Cl-:1].[Hf+4:5]

참가 물질

4

반응물 3

HCID 1140TolueneHCID 139759Lithium, mol. (Li2)HCID 9927068Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)-

생성물 1

HCID 21904050Cyclopenta-1,3-diene;hafnium(4+);dichloride

실험 절차

1.81 g (5.65 mmol) of hafnium tetrachloride are added to a suspension, cooled to -78° C., of 2.00 g (5.64 mmol) of the dilithium salt (Example 4) in 150 ml of toluene. The orange suspension is allowed to warm to room temperature, and is stirred for a further 2 days in order to complete the reaction. Insoluble constituents are then filtered off via a frit, and the orange-red filtrate is evaporated to dryness on an oil pump. 30 ml of pentane are added to the orange-red residue, and the mixture is stirred vigorously overnight. Removal of the solvent in vacuo gives the hafnocene dichloride as beige powder in a crude product yield of 700 mg (24%). The 1H-NMR spectrum of the crude product shows only one diastereomer.

후처리

  1. customthe reaction
  2. filtrationInsoluble constituents are then filtered off via a frit
  3. customthe orange-red filtrate is evaporated to dryness on an oil pump
  4. addition30 ml of pentane are added to the orange-red residue
  5. stirringthe mixture is stirred vigorously overnight
  6. customRemoval of the solvent in vacuo

출처 및 근거

ORD 기록
ord-dc46f464170347aa959b35008bd9528f
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990254

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