Ruthenium(III) chloride hydrate

01 Nov.,2023

 

76.3% In methanol; EXAMPLE 1 Synthesis of (2,4-dimethylpentadienyl) (ethylcyclo-pentadienyl) Ruthenium and Heat Decomposition Properties Thereof 400 g of zinc was weighed into a four-necked flask. After purging the container with argon, 205 ml of 2,4-dimethyl-1,3-pentadiene was added thereto to give a suspension. Then a solution of 30 g of ruthenium trichloride n-hydrate (n: about 3) dissolved in 1000 ml of methanol was dropped thereinto at room temperature over 40 minutes. After the completion of the dropping, the mixture was stirred at room temperature for 30 minutes, then heated to 60 C. and stirred for additional 2 hours. The mixture was once cooled by allowing to stand and then 12 ml of ethylcyclopentadiene was added thereto. The resultant mixture was stirred as such at room temperature for 30 minutes, then heated to 60 C. and stirred for additional 2 hours. After the completion of the reaction, the mixture was cooled to room temperature and the unreacted zinc was removed with the use of a glass filter. Next, it was extracted with hexane (750 ml*1, 300 ml*4). The extracts were concentrated under reduced pressure and the oily product thus obtained was distilled under reduced pressure to thereby give 25.4 g of target (2,4-dimethylpentadienyl) (ethylcyclo-pentadienyl) ruthenium (yield: 76.3%). Oily yellow product: 1H-NMR (500 MHz, CDCl3, deltappm) 5.38 (s, 1H), 4.63 (t, J=2.0 Hz, 2H), 4.52(t, J=2.0 Hz, 2H), 2.70 (d, J=2.5 Hz, 2H), 2.15 (q, J=7.5 Hz, 2H), 1.93 (s, 6H), 1.12 (t, J=7.5 Hz, 3H), -0.09 (d, J=2.5 Hz, 2H) IR (neat, cm-1)

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