EXP260

=Researcher= Matthew McBride =Objective= To determine the solubility of 4-chlorobenzaldehyde in ethanol at 1C and 25C and characterize any product formed using SAMS HNMR method. =Procedure= Two saturated solutions of 4-chlorobenzaldehyde were created and warmed in a 45C water bath. One solution was then placed in a 25C bath and the other was placed in a 1C bath. The supernatant of each solution were anazlyzed by 500Hz HNMR to determine solubility. Any crystals formed were analyzed for possible hemiacetal formation. =Results= [|SAMS Sheet] **[Fix permissions JCB]** =Discussion= =Conclusion= =Log=
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2012-02-15
10:20 Filled a beaker with water and placed it on a hot plate to create a 45C water bath. 10:29 3.4295g of 4-chlorobenzaldehyde was weighed out and placed in a 20mL glass test tube labeled Tube 1. 10:32 3.0296g of 4-chlorobenzaldehyde was weighed out and placed in a 20mL glass test tube labeled Tube 2. 10:38 Ethanol was added to each test tube to create an approximately 1:1 ratio of 4-chlorobenzaldehyde to ethanol solution. The test tubes were sealed with parafilm, inverted several times and placed in the 45C water bath. 10:40 Solid was observed on the bottom of each test tube, so each tube was inverted several times to throughly mix the solutions. 10:43 A 25C water bath was created. No solid was visible in either test tube. 10:44 Placed Tube 1 in the 25C water bath. 10:54 No crystals were visible in Tube 1. 10:59 Added Tube 2 to a 4C ice bath. 11:06 White crystals were visible in Tube 2 in the ice bath. Temperature of the ice bath was at 1C. 11:14 Suction filtration with a Buchner funnel was set up. 11:15 No crystals were visible in Tube 1 in the 25C water bath. 11:21 Tube 2 was removed from the 1C ice bath and the thick crystal solution was scraped out of Tube 2 onto the Buchner funnel. 11:22 An empty vial was weighed to be 4.7201g. 11:23 The crystals (white, fluffy looking) were left on the filter paper with suction applied to the funnel to dry the crystals. 11:26 The suction was disabled and the dried crystals were scraped from the filter paper to the vial. A small amount of the crystals were lost during this exchange, because a few of the crystals were not captured by the vial. 11:34 The weight of the vial with the crystals was 5.5884g.