CRSEXP012

=Researcher= Cuepil Choi =Objective= To see if carrying out CRSEXP006 with a benzene ethylene glycol azeotrope and benezene water azeotrope in a rotary device with suction could help isolate and crystalize the acetal products. =Procedure= Ethylene glycol and 4-chlorobenzaldehyde were mixed in a 1.2:1 ratio, respectively, in a 100 mL round flask. Enough benzene was added to the round flask until approximately 30 mL of solution was inside. The round flask was clamped onto a rotary device. Rotary device was turned on and weak suction applied. When most of the top benzene layer escaped the round flask into the second chamber, additional benze was added. Samples were taken every time benzene was added after mixing through the rotary device. =Results=
 * Aborted**

=Conclusion= HNMR spectra showed little acetal production. Rotary device did not produce desirable results and further benzene additions were aborted. =Log=

2013-07-26
11:20 mass of 100 mL round flask 1 65.193 g 11:24 1.081 g 4-chlorobenzaldehyde added to round flask 1 11:25 2.211 g ethylene glycol added to round flask 1 11:27 0.276 g g 4-chlorobenzaldehyde added to round flask 1 11:30 10.175 g of benzene added to round flask 1 11:35 two layers formed, S-1 taken from top benzene layer after mixing by rotating the rotary device 11:52 clear benzene layer goes cloudy 11:58 rotary device reaches 55 C upper round flask of rotary device starts to have a clear liquid 12:00 60 C reached on rotary device 12:19 rotary device turned off 12:22 10.085 g benzene add to round flask 1 12:26 rotary device back on 12:27 S-2 taken from top benzene layer 12:29 64 C reached on rotary device 12:34 top round flask on rotary device starts to have clear liquid 12:39 rotary device turned off 12:48 8.617 g of benzene added 12:53 S-3 taken from top benzene layer 13:30 HNMR spectrum 1 taken of S-1 13:50 HNMR spectrum 2 taken of S-2 13:56 HNMR spectrum 3 taken of S-3