[awais]

Dear Friends
I m synthesizing the sulfur compounds, cyclo and straight chain. I have problem in seperating the organic layer after washing with water. It becomes homogenous, sort of emulsion. I had tried the techniques like salt additin but no positive effect. Can anybody help me??

Thanks in advance

[barcrphd]

what is your compound and what is the organic solvent that you are using?

[awais]

im using dichloromethane and , molecule is cyclo polysufide with methylene groups. The dichloromethane is a reactant as well in this case

[barcrphd]

write the complete reaction. starting material, reagent and conditions. that may help to choke out the work up procedure.

[awais]

Na2 S2.5 + S + H2O + CH2Cl2--------- Lenthionine [CH2]2 S5
The methylene chloride is active reactant as well and solvent. After 7 hrs stirring there are 2 layers observed. The organic layer seperated and while washing this organic layer with water, the seperation of water is not possible, coz i ve to remove water and then after drying with mgso4 the excess of solvent is evaporated, the remaining oily liquid gives crystals at room temp.

Now my compound is in all this mixture, if i wash , i can't seperate organic layer.

[barcrphd]

your post confuses me more.
what is this Na₂S_2.5? did you mean Na2 S? then you are using water and dichloromethane at the start of the reaction. then and there itself you should get two layers no? but your post suggests you are getting two layers only after 7 hours? what are these two layers, water and dichloromethane? and are both the layers clear?
please make as clear as possible...

[awais]

Dear
The reaction is that u take sodium sulfide nonahydrate and sulfur in water(to make stichiometric ratio as Na2S2.5), and adjust the ph with H2S at 8 , at this Ph u add methylene chloride, at the end of 7 hrs u get two layers , one organic down opaque color and other orange color as upper layer.
in orgaanic layer when u evaporatee the solvent oily material is obtained which on standing at room temp goes to crystals, but in my case its not like this.
i think this ratio of Na2S2.5 is not balanced otheerwise reaction is ok.