purification of organic compound

[hithendra p.v.]

As part if our research project work we had to synthesize m-nitro acetophenon. we used acetophenon and nitrated it with nitrateing mixture the product m-nitro acetophenon which we optained is a sticky mass it is some what oily we repeatedly washed the mass and also recrystallized it in ethanol but we are unable to get rid of the stickyness an not able to get crystals, it still forms lumps or sticky mass please help me out project has come to a stand still please suggest a technique to purify this compound. i am an under graduate student and working with minimum lab facilities.

[UC]

Always check the synthetic literature first- http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=cv2p0434

 

I suggest you take the current product and treat it as in the second paragraph and on, scaling portions for your amount of product.

 

It looks to be rather conditions-sensitive. You may want to re-run the procedure using the recommendations there in order to minimize difficult-to-seperate side products.

[Capita]

It sounds like an impurity issue... usually oily substances means something was done wrong in the lab like unclean glassware, over/under heating or improper procedures.

[hithendra p.v.]

Thank you UC and Capita for replying , I did check the literature from http://www.orgsyn.org but the procedure was not exactly right we had to conduct many trials in order to synthesise the sticky mass after which i followed the same procedure to purify the product but in vain. i should agree that the stickyness did reduce but crystalization did not take place. some people advised me to use the roter but i don't have access to those instruments. please direct me to a valid procedure that can help me purify the m-nitroacetophenone.