CRSEXP028

=Reseracher= Cuepil Choi =Objective= To see whether recrystallizing 4-chlorobenzaldehyde ethylene glycol acetal in ethanol is a practical preparatory procedure. =Procedure= 4-chlorobenzaldehyde was added to a 10 mL screw cap test tube with roughly 1:1.5 mole ratio between 4-chlorobenzaldehyde and ethylene glycol. Mixture was refluxed in a 30 mL erlenemeyer flask filled with an ethylene glycol bath. =Results= (experiment aborted) =Discussion= Experiment was aborted due to time constraint and problems mentioned in the conclusion. =Conclusion= Due to time constraints, the NMR machine's trouble finding z0, and adding too much ethanol, experiment was aborted. =Log=
 * Experiment Aborted**

2013-10-10
11:42 20 mL screw cap test tube 1 mass recorded as 9.8228 g (without the cap, after taring a 30mL erlenmeyer flask) 11:45 0.1607 g 4-chlorobenzaldehyde from stock bottle #0941-0 added to test tube 1 11:47 0.1852 g of ethylene glycol added to test tube 1 11:50 30 mL erlenmeyer flask filled with ethylene glycol and test tube 1 was placed inside ethylene glycol bath 11:51 hot plate heat setting set to 250 C 11:58 4-chlorobenzaldehyde has melted, sample S-1 taken. mixture immediately solidifies 12:11 temperature of bath recorded at 146 C with lazer gun 12:50 NMR sample taken 13:10 test tube 1 take out of bath 13:11 ~.25 ml of ethanol added to test tube 1. 13:21 test tube put in dry ice and acetone bath 13:40 NMR machine having trouble finding z0. Due to time constraints, aborted.

2013-10-11
13:53 **[I don't see an Erlenmeyer on a hot plate with a test tube inside being heated - so what happened after 11:58 the previous day? JCB]**