Exp033

== =Objective:= To distill [|butyraldehyde].

=Procedure:=

Added [|butyraldelhyde] to a 100ml round bottom flask and attached a thermometer to monitor temperature. Placed round bottom flask in a heating mantle. Attached a condenser to the round bottom flask and added another 100ml round bottom flask to condenser (collection flask). Placed collection flask in an ice bath and attached apparatus to a ring stand. Turned on medium heat and allowed butyraldehyde to slowly boil for 3 hrs.

=Results= //**20mL**// [|HMR] CH3 peak at 0.5ppm CH2 peak at 2.4ppm CH2-CO peak at 2.1ppm Aldehyde proton peak at 9.6 Carboxylic acid bump at 10.8ppm

=Discussion=

The integration of the aldehyde peak (5.23) is incorrect based on integration of the aliphatic protons (28.44, 25.22, 39.15). The presence of a bump also indicates that a carboxylic acid is present.

=Conclusion:= Based on the information above it is determined that the aldehyde is impure. For future distillations it would be recommended to set up apparatus under nitrogen atmosphere.

=Log:=

2006-10-22
12:30 Set up distillation apparatus. Allowed 30mL butyraldehyde to boil slowly for 3 hrs while stirring on medium heat (setting 3). Condensation was noticed at approximately 12:50 at a temperature of 85C. =Tags= [|Butyraldelhyde]InChI=1/C4H8O/c1-2-3-4-5/h4H,2-3H2,1H3

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