tert-Butanol → HCID 178454921, compound

HRID 2229860Notes

Reaction equation

HRID 2229860 reaction equation
[CH:1]1([Ru:6][CH:7]2[CH:11]=[CH:10][CH:9]=[CH:8]2)[CH:5]=[CH:4][CH:3]=[CH:2]1.[Cl-].[Al+3].[Cl-].[Cl-].[C:16](O)([CH3:19])([CH3:18])[CH3:17]>O>[C:16]([Ru:6]([CH:1]1[CH:2]=[CH:3][CH:4]=[CH:5]1)[CH:7]1[CH:11]=[CH:10][CH:9]=[CH:8]1)([CH3:19])([CH3:18])[CH3:17]

Participants

5

Reactant 3

HCID 6386tert-ButanolHCID 6451240Aluminum(III) ChlorideHCID 178420581HCID 178420581, compound

Product 1

HCID 178454921HCID 178454921, compoundYield 20%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
120 °C

Procedure

8.0 g of bis(cyclopentadienyl)ruthenium, 3.0 g of aluminum chloride, and 80 g of polyphosphoric acid were mixed. The mixed solution was heated to 100° C. under a nitrogen atmosphere, to which 3.0 g of tert-butyl alcohol was added dropwise over 30 minutes, and then the mixture was heated to 120° C. to carry out the reaction for 4 hours. After the reaction, hot water was added to the solution to remove polyphosphoric acid, and then distillation treatment gave 2.0 g of tert-butylcyclopentadienyl(cyclopentadienyl)ruthenium. Five lots of tert-butylcyclopentadienyl(cyclopentadienyl)ruthenium were prepared by this preparing method, and subjected to film production as described later.

Workup

  1. additionwas added dropwise over 30 minutes
  2. customthe reaction for 4 hours
  3. additionwas added to the solution
  4. customto remove polyphosphoric acid
  5. distillationdistillation treatment

Sources & evidence

ORD record
ord-fe9da51f223e489fa601e37f99e85377
Source dataset
uspto-grants-2002_07
Patent number
US06420582B1

Reaction notes

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