Chromic Cation → Aluminum

HRID 1764081Notes

Reaction equation

HRID 1764081 reaction equation
[Cr+3:1].[CH3:2][CH:3]([CH2:5][CH3:6])[O-:4].[Al+3:7].[CH3:8][CH:9]([CH2:11][CH3:12])[O-:10].[CH3:13][CH:14]([CH2:16][CH3:17])[O-:15]>ClCCl>[CH3:2][CH:3]([CH2:5][CH3:6])[O-:4].[Al+3:7].[CH3:8][CH:9]([CH2:11][CH3:12])[O-:10].[CH3:13][CH:14]([CH2:16][CH3:17])[O-:15].[Al:7].[Cr:1]

Participants

6

Reactant 2

HCID 27668Chromic CationHCID 61289Aluminum sec-butoxide

Product 3

HCID 23976ChromiumHCID 61289Aluminum sec-butoxideHCID 5359268AluminumYield 3.7%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

As indicated, in some cases the catalyst was also coated with an aluminum alkoxide. In these cases, dichloromethane is added to a similar flask as used in step B and while maintaining a nitrogen atmosphere stirring is commenced (see U.S. Pat. No. 3,984,351 incorporated herein by reference). To the flask is added a portion of the supported hydrated polymeric chromium (III) of step B. A solution of dichloromethane and aluminum sec-butoxide is prepared in a pressure equalizing dropping funnel and the funnel attached to the stirred flask. The aluminum sec-butoxide solution is gradually added to the flask at the rate of 10 grams of solution per minute. After the addition of the solution is complete the slurry in the flask is stirred for about 1 hour. The supernatant liquid is removed by filtration or distillation at reduced pressure and the coated gel is dried in a rotary evaporator at temperatures up to about 60° C. and 29 inches Hg vacuum. The aluminum sec-butoxide was absorbed to provide about 3.7% aluminum by weight of the support (atomic ratio of aluminum to chromium of 8/1). Where indicated, a portion of the supported hydrated polymeric chromium (III) compound of step B was heat aged in chloroform in the presence of poly(di-μ-diphenylphosphinatotitanium dichloride) with an atomic ratio of titanium to chromium of 1/1; and another portion of the supported anhydrous polymeric chromium (III) of step B was heat aged in chloroform in the presence of aluminum sec-butoxide (atomic ratio of aluminum to chromium of 4/1).

Workup

  1. temperaturewhile maintaining a nitrogen atmosphere
  2. additionAfter the addition of the solution
  3. stirringis stirred for about 1 hour
  4. customThe supernatant liquid is removed by filtration or distillation at reduced pressure
  5. customthe coated gel is dried in a rotary evaporator at temperatures up to about 60° C.
  6. customThe aluminum sec-butoxide was absorbed

Sources & evidence

ORD record
ord-2c07954204e747a8bc7703f5df725c11
Source dataset
uspto-grants-1978_09
Patent number
US04115318

Reaction notes

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