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★ ★ ★ 小木虫(金币+0.5):给个红包,谢谢回帖交流 ^_^@^_^(金币+2,VIP+0):哈哈,应助非常到位! 6-15 11:27
国内有不少单位卖,如陕西开达
如果想自己合成
可以参考Inorganic Syntheses,. 1972, 13, 92.
The early preparations gave poor yields but highly efficient
methods have been developed recently. Optimum yields are
obtained by the method of Pino and his coworkersg in which
tris(2,4-pentanedionato)ruthenium(III) is treated with equimolar
mixtures of hydrogen and carbon monoxide at moderate
temperatures and pressures ( 140-160°, 200-300 atmospheres).
However, this method is limited by the availability of the tris-
(2,4-pentanedionato)ruthenium(III) which is obtained in only
low yields from the readily available ruthenium trichloride
hydrate. The method given here is a modification on the Pino
method.
Reactions are carried out in a 1 L. autoclave capable of withstanding
pressures up to 300 atmospheres and operating at
maximum temperatures of 300°. All solvents must be freshly
distilled before use and all manipulations carried out in a wellventilated
hood. It is essential that the sodium acetylacetonate,
(2,4-pentanedionato)sodium, be freshly prepared before use. *
Ruthenium trichloride hydrate (5 g.), sodium acetylacetonate
(7 g.), and methyl alcohol (140 ml.) are placed in the autoclave
in that order. Hydrogen (40 atmospheres) and carbon monoxide
(120 atmospheres) (i.e., total initial pressures = 160 atmospheres
at room temperature) are then added and the reaction mixture
heated at 165" for 4 hours. When cold the pressure is released
and the crude orange crystalline dodecacarbonyltriruthenium
separated by filtration. The mother liquor is evaporated to
dryness and any additional product extracted into hot hexane
in a Soxhlet apparatus. The combined products are then
recrystallized from hot hexane. t Yields vary slightly from
preparation to preparation but are usually in the range 50-55 yo
(2.5 g.). (The checker obtained a yield of 3.0 g., 70%.)
[ Last edited by mland on 2009-6-12 at 11:13 ] |
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