User:Ellen Petersen/Notebook/MOF/2013/06/25

MOF

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DPNI: 06-25-13 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 .8051 g of 1,4,5,8 Naphthalenetetracarboxylic dianhydride, and .8481 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 56, switch down accordingly until it reaches 135 degrees consistently. 9.) If solution seems to be boiling adjust and turn down 10.) Solution stable at 134 degrees at 50, mark red line on it to see difference in solution level. ______________________________________________________________________________________________________ 06-26-13 11.) Turn off nitrogen and water, Cool to Room Temperature 12.) Pour solution onto 600 mL of diethyl ether 13.) Filter out solid