HCID 178478629, compound → HCID 178420587, compound

HRID 1452683Notes

Reaction equation

HRID 1452683 reaction equation
[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

Participants

5

Reactant 2

HCID 178478629HCID 178478629, compoundHCID 178506658HCID 178506658, compound

Product 1

HCID 178420587HCID 178420587, compound

Reagents, catalysts & solvents 2

HCID 1140TolueneSolvent2×HCID 3283Diethyl EtherSolvent2×

Procedure

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%).

Workup

  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%)

Sources & evidence

ORD record
ord-ace58e12ebd34ad88077113332fc73a7
Source dataset
uspto-grants-2009_01
Patent number
US07473745B2

Reaction notes

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