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DPNI: 06-26-13
- 1.) Add solids 1,4,5,8 Naphthalenetetracarboxylic dianhydride (.805 g, 3.00 mmol) and 4-aminopyridine (.847 g, 6.00 mmol)to round bottom flask (I added .8054 g of 1,4,5,8 Naphthalenetetracarboxylic dianhydride, and .8479 g of 4-aminopyridine)
- 2.) Add 150 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 50, switch down accordingly until it reaches 135 degrees consistently.
- 9.) If solution seems to be boiling adjust and turn down
- 10.) Solution stable at 135 degrees at 35, mark red line on it to see difference in solution level.
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06-27-13
- 11.) Turn off nitrogen and water, Cool to Room Temperature
- 12.) Not enough diethyl ether, took 400 mL of diethyl ether (instead of the required 600 mL) and poured 2/3's of DPNI solution into the 400 mL of diethyl ether.
- 13.) Filter out
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07-02-13
- 14.) Ran 1/4 of the DPNI with 150 mL of ethanol through the rotavap
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MOF
