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Thursday, April 15, 2010

Preparation of RuCl(dppe)Cp

ref: A.G Alonso and L.B Reventos, J.Organomet.Chem.,1998, 338, 249

RuCl(PPh3)2Cp -------------------> RuCl(dppe)Cp
0.277g dppe
100 ml toluene

  1. Set up the apparatus. See synthesis of RuCl(PPh3)2. (mass of RuCl(PPh3)2Cp used = 0.5085g)

  2. The yellowish solution was let to reflux for about 6 hours
  3. Next, follow the crystallization step (see previous page)

  4. The filtrate volume was reduced to ~20 ml by rotavap

  5. n-hexane was added into the solution (in excess)
  6. Leave the solution which now contains precipitate in freezer for ~20 mins to allow the ppt. to settle down

  7. Filter again using vacuum suction

  8. The deposited ppt. at the RBF was scratched off using spatula

  9. Combine all the products obtained and store in vial

RuCl(dppe)Cp

percentage yield = 46%

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