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二茂铁(102-54-5)的分离

2014-08-04 来源:亚科官网

 1 with samples

Take the rough product 20mg placed in dry small beaker, adding ethyl acetate dissolved, add about 200mg silica gel, evenly stirring to obtain slurry, an infrared lamp drying to obtain granular loose.
2 wet packing
3 elution
First used by ether / ethyl acetate as eluent from the capital to join =20/1, elution speed control in 1-2 drops per second, gradually get yellow chromatographic band. Two yellow Mao was first out from under the column, collecting the eluting solution with the conical flask dry. When the yellow Pu Dai completely eluted with petroleum ether, ethyl acetate / =1/5 eluent, and orange red band edge, the orange red Pu Dai completely eluted, eluent is collected by another has dry conical flask. 4 collection of products
The eluate is collected yellow raw two ferrocene has not completely reacted: orange red in the eluate is the main product of two acetyl ferrocene. The orange red eluent into the dried eggplant shape bottle has been weighing, rotary evaporation from solution with ethyl acetate, get the product, the product aubergine bottle to the evaporating dish has weighed in, finally get the beautiful crystal orange red. And summarize the experimental discussion: acetyl two ferrocene in this experiment is the preparation of basic failure, no obvious difference products paper chromatography with the original product, reason should be the container with water vapor, the ethyl acetate is hydrolyzed, the product is little. M (two =0.06g acetyl ferrocene)
The results of column chromatography to yield of m=0.0121g w=60% last measuring melting point: ketal initial melting point =60 ℃ final melting point =63 ℃
Cinnamic acid initial melting point =131 ℃ final melting point =135 ℃ glycol initial melting point =136 ℃ final melting point =139 ℃


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