HCID 178478629, Verbindung → HCID 178420587, Verbindung

HRID 1452683Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1452683
[C:1]1([Li])[CH:16]=[CH:15][CH:14]=[C:13]2[C:2]=1[CH:3]=[C:4]1[C:12]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]=[C:5]12.[Cl-:18].[Cl-].[Cl-].[CH:21]1([Zr+3:26])[CH:25]=[CH:24][CH:23]=[CH:22]1>C1(C)C=CC=CC=1.C(OCC)C>[Cl-:18].[Cl-:18].[C:1]1([Zr+2:26][CH:21]2[CH:25]=[CH:24][CH:23]=[CH:22]2)[CH:16]=[CH:15][CH:14]=[C:13]2[C:2]=1[CH:3]=[C:4]1[C:12]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]=[C:5]12

Komponenten

5

Edukt 2

HCID 178478629HCID 178478629, VerbindungHCID 178506658HCID 178506658, Verbindung

Produkt 1

HCID 178420587HCID 178420587, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittel2×HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A sample of the indeno[1,2-b]indolyl lithium salt produced above (10 g, 42 mmol) is dissolved in toluene (95 mL) to produce an orange slurry. Diethyl ether (35 mL) is added slowly to give an orange solution. This solution is added over 15 min. at room temperature with stirring to a slurry of cyclopentadienylzirconium trichloride (11 g, 42 mmol) in toluene (190 mL) and diethyl ether (190 mL). The mixture turns deep red and is kept at room temperature overnight. The slurry is filtered to recover a red solid, which is washed with toluene (200 mL) and dried under vacuum to give the catalyst (16.5 g, 78%).

Aufarbeitung

  1. customto produce an orange slurry
  2. customto give an orange solution
  3. additionThis solution is added over 15 min. at room temperature
  4. filtrationThe slurry is filtered
  5. customto recover a red solid, which
  6. washis washed with toluene (200 mL)
  7. customdried under vacuum
  8. customto give the catalyst (16.5 g, 78%)

Quellen und Nachweise

ORD-Eintrag
ord-ace58e12ebd34ad88077113332fc73a7
Quelldatensatz
uspto-grants-2009_01
Patentnummer
US07473745B2

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