Question Help!! naphthonyl indole

charmingcho

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I made naphthonyl indole, but it's too sticky

What kind of solvent should be used for recrystalization to obtain high purity?
 

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billian1

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A good solvent for crystallization should have high solubility for the solute as well as high potential recovery. This means that the solvent for cooling crystallization should be such that it should have high solubility for the solute at a high temperature, and relatively low solubility at a low temperature (i.e. high temperature coefficient of solubility). Initial solubility determines the size of the crystallizer, while the temperature coefficient of solubility determines the yield. In the case of drowning out crystallization the solvent should have high solubility for the solute, while the solubility should decrease greatly when the anti-solvent is added. Eqn's 2 and 3 can be used to evaluate the potential recovery for cooling and drowning out crystallizations respectively. If you might need any help or change your mind to order just PM mee directly okey
 

G.Patton

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Hello, I don't understand sequence of your manipulations in your picture. Did you add Na2SO4 into the mixture of organic and water layers?

Tip:
SolubilityVery soluble in N,N-Dimethylformamide, Soluble in methanol, Sparingly soluble inglacial acetic acid, Very slightly soluble inchloroform, Practically insoluble in water.
  • DMF: 30 mg/ml
  • DMSO: 30 mg/ml
  • DMSO: PBS(pH 7.2) (1:2): 0.3 mg/ml
 

charmingcho

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Thank you for answer. First, water was separated with a separation funnel and dry solution(using Na2SO4) was evaporated, but it was sticky.

second, Na2SO4 was added to a solution in which water and EA were not separated, and an EA layer was obtained above and a solvent was evaporated. It's same sticky.

Are you saying that it is good to use DMF for solvent when recrystalization?
 

G.Patton

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Probably your product is spoiled. You can try to add a little bit solvent (DMF or chloroform), heat a mixture, pour onto a Petri dish and scratch by glass rod. You have to let to a solvent evaporates slowly. A scratching procedure makes crystallization centers.
 
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