Exp279

=Researcher= Mark Mangir

=Results= [|Mass and Yield Calculations]

[|NMR Spectra]


 * [|Sample Characterization]**

=**Discussion**= All of the washed spectra showed the desired Imine compound, not the acid as previously obtained by Evan. This means this is a proper procedure. The compound is very soluble in the ethanol wash, so the yield is highly dependent on how much ethanol is used to wash the sample.

=Log=

2012-03-05
13:30 Added 2.488g of 4-chlorobenzaldehyde to a 20mL screw cap test tube (Tube 1). Added 10mL of ethanol to vial 1. 13:40 Added 1.244g of 4-chlorobenzaldehyde to a 20mL screw cap test tube (Tube 2). Added 10mL of ethanol to vial 2.

13:50 Added 1.244g of 4-chlorobenzaldehyde to a 20mL screw cap test tube (Tube 3). Added 10mL of ethanol to vial 3. 14:00 Added 1.244g of 4-chlorobenzaldehyde to a 20mL screw cap test tube (Tube 4). Added 10mL of ethanol to vial 4 14:10 Added 10mL of ethanol to a 20mL screw cap test tube (Tube 5). 14:12 Added 0.830g of aniline to tube 1. 14:14 Added 0.829g of aniline to tube 2. 14:16 Added 1.664g of aniline to tube 3. 14:18 Added 0.832g of aniline to tube 5.

2012-03-07
12:30 Took 200 uL samples from tubes 1-3 and placed them in NMR tubes. Sample two solidified in the pipette, and would not transfer into the tube. Also, immediately after being disturbed vial two solidified. 12:40 Tubes 1 and 3 also solidified, and their NMR samples formed a large amount of precipitate. 12:50 Used pipette to mix tube 2, and it became a slush, vacuum filtered it and took a sample of the unwashed precipitate (Sample 2 Unwashed). 13:00 Washed the precipitate with 5mL of ethanol, let dry, and took another sample (Sample 2 Washed). 13:10 Prepared NMR samples of the unwashed, washed, and filtrate from sample 2 in CDCl3. Ran samples on 500MHz NMR. Files for the three samples prepared from sample 2. mimEXP279_unwashed_precipitate_1-1.jdx mimEXP279_washed_precipitate_1-1.jdx mimEXP279_filtrate_1-1.jdx

2012-03-09
12:30 Vacuum filtered Sample 1. Washed Precipitate with 5mL of ethanol. 12:40 Transferred washed sample (Sample 1 Washed), into a pre-weighed vial. 12:50 Parafilmed Sample 1 Washed and Sample 2 Washed and placed in a vacuum desiccator to dry. 13:20 Vacuum filtered Sample 3. Washed Precipitate with 5mL of ethanol. 13:30 Transferred washed sample (Sample 3 Washed), into a pre-weighed vial. 13:35 Parafilmed Sample 3 Washed, poke a hole in the parafilm, and placed in a vacuum desiccator to dry.

2012-03-14
13:00 Prepared NMR Samples for Washed Samples 1-3 prepared on 03-09 in CDCl3. Ran the samples on the 500 MHz NMR. Sample 1- mimEXP279_washed_precipitate_1-2.jdx Sample 2- mimEXP279_washed_precipitate_2-2.jdx Sample 3- mimEXP279_washed_precipitate_3-2.jdx