My 1st synthesis (12 April 2010) - chloro(cyclopentadienyl)bis(triphenyl-phosphine)ruthenium(ii)

Title : Preparation of RuCl(PPh3)2Cp

Procedure

ref: Chloro(η5-Cyclopentadienyl)Bis(Triphenyl-Phosphine) Ruthenium(II): Rucl(PPh3)2(η5-C5H5)Inorganic Syntheses: Reagents for Transition Metal Complex and Organometallic Syntheses, Volume 28 , Pages270 - 272.
M. I. Bruce, C. Hameister, A. G. Swincer, R. C. Wallis, S. D. Ittel
Copyright © 1990 Inorganic Syntheses, Inc

i. Distillation of diCp -> Cp




Make sure!!

• to purge the apparatus with N2 before start distilling
• no leaking
• to attach the water inlet while distilling
• do not use water bath for the distillation, use Silicon oil instead as water can easily evaporated
• the receiver flask must be attached to an ice-containing beaker (to prevent the product to get polymerized back to diCp)
  

ii. synthesis of RuCl(PPh3)2Cp

First of all, set up the vacuum line since the compounds we are dealing with are air-sensitive.

the complete set-up of vacuum line for my bench is shown. Well, bit of messy but as long as you understand the flow, you will get it (i'm still learning).

Make sure!!

• only open the intended use of N2 inlet
• to always check for any leak of the system
• always REMEMBER to remove the N2 cylinder from the system when not in use

Next, we can start to assemble the apparatus for the synthesis. (see next)