User:Andrew W Long/Notebook/Synthesis of Lipid Modulators/2015/10/02: Difference between revisions

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Procedure for large-scale rxn:
Procedure for large-scale rxn:
#Calculations:
#Calculations:
##Start with mass of CNP and get moles of CNP:  
##Start with mass of CNP and get moles of CNP:                                                                         <math>\frac{250mg}{1}|\frac{1g}{1000mg}|\frac{1mol}{158.54g}=0.00158mol</math>  
 
<math>\frac{250mg}{1}|\frac{1g}{1000mg}|\frac{1mol}{158.54g}=0.00158mol</math>  
##Get mass of MTT using moles of CNP (use 5% extra MTT since it is less valuable): <math>\frac{Xg}{1}|\frac{1mol}{164.27g}=1.05*0.00158mol=0.001659mol</math>  
##Get mass of MTT using moles of CNP (use 5% extra MTT since it is less valuable): <math>\frac{Xg}{1}|\frac{1mol}{164.27g}=1.05*0.00158mol=0.001659mol</math>  


Revision as of 16:04, 5 October 2015

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Purification of Product of Rxn Between MTT and CNP, and Large-Scale Reaction Setup

Note that MTT refers to 5-(methylthio)-1,3,4-thiadiazole-2-thiol, and that CNP refers to 2-chloro-3-nitropyridine. Structures shown here

Goals:

  • To purify the products of my second reaction (Ross carried it out with the modified procedure).
  • To set up a large-scale version of the previous small-scale reaction. Target compound must be synthesized and purified by Wednesday (10/07/15)

Procedure for purification:

  1. The product was shown to be slightly soluble in ethyl acetate (which is more polar than dichloromethane). The insoluble impurity could be the result of residual triethylamine. A "dirty column" was run in an attempt to remove the impurity.
    1. The column was a Büchner funnel containing powdered silica, which sat in a vacuum flask.
    2. The powdered silica was then made into a slurry with hexane.
    3. The compound, once redissolved in methanol, was run through the column. It was hoped that the triethylamine would remain in the silica.
    4. After the fraction collected with ethyl acetate was obtained, another flask was used to collect a methanol fraction.
  2. Mass spectrometry was used to examine the two fractions. The result is shown below:

Procedure for large-scale rxn:

  1. Calculations:
    1. Start with mass of CNP and get moles of CNP: [math]\displaystyle{ \frac{250mg}{1}|\frac{1g}{1000mg}|\frac{1mol}{158.54g}=0.00158mol }[/math]
    2. Get mass of MTT using moles of CNP (use 5% extra MTT since it is less valuable): [math]\displaystyle{ \frac{Xg}{1}|\frac{1mol}{164.27g}=1.05*0.00158mol=0.001659mol }[/math]


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