User:Ellen Petersen/Notebook/MOF Continued/2013/04/02

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DPNI

  • 1.) Add solids 1,4,5,8 Naphthalenetetracarboxylic dianhydride (.4025 g, 3.00 mmol) and 4-aminopyridine (.4235 g, 6.00 mmol)to round bottom flask
  • 2.) Add 75 mL of solvent (DMA) ~keep under hood~
  • 3.) Add Stir Bar to solution
  • 4.) Put under spout and raise black knob until there is enough pressure to hold it in place
  • 5.) Begin to stir
  • 6.) If attached to condenser, turn on water very slightly
  • 7.) Turn on nitrogen: ensure bubbles are about 1 every 4 seconds. (Turn little end of nossle up)
  • 8.) Turn on heat to 40, switch down accordingly until it reaches 135 degrees consistently.

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04-03-13

  • 9.) Turn off nitrogen and water, Cool to Room Temperature
  • 10.) Filter out solid using diethyl ether
  • 11.) NMR in Chloroform (See Image Below)