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ChemicalBook CAS DataBase List OSMIUM CARBONYL
15696-40-9

OSMIUM CARBONYL synthesis

5synthesis methods
20816-12-0 Synthesis
Osmium tetroxide

20816-12-0
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$22.39/2ML

201230-82-2 Synthesis
carbon monoxide

201230-82-2
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Yield: 83%

Reaction Conditions:

at 175; under 30003 - 90009 Torr; for 10 h;

Steps:


5.0 g (20 mmol) of osmium tetraoxide and 70 ml of anhydrous methanol(freshly distilled from magnesium turnings) were placed in a 250 ml autoclave. Carbon monoxide (CP grade) was filled in to pressure of 40 bars, and then purged to remove the air inside. It was then refilled up to 80 bars and the reaction mixture was heated at 175°C with vigorously stirring for 10 h. During the heating process, the pressure for the reaction system was about 120 bars. After heating was stopped, the autoclave and its contents were allowed to cool down naturally to room temperature before the remaining carbon monoxide gas was purged (about 12 hours needed). The autoclave was then opened to reveal bright yellow crystals of dodecacarbonyl triosmium suspended in a yellowish-green solution. The products were separated by filtration and washed with ice cold methanol twice and then dried under a slow stream of nitrogen and finally under a vacuum (5.0 g, yield 83 %). The obtained product was characterized by IR spectroscopy[0113] IR (v CO) in CH2Cl2: 2068(s), 2034(s), 2013(w), 2000(w) cm"1.

References:

NATIONAL UNIVERSITY OF SINGAPORE WO2008/127197, 2008, A1 Location in patent:Page/Page column 37

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