Wednesday, May 31, 2006

Exp 012

To convert adrenaline to a catechol aldehyde using acid catalysis. How this fits into the synthesis of anti-malarials is described here.

Adrenaline (227 mg, 1.239 mmol) was added to a 100mL round bottom flask that holds a thermometer with concentrated sulfuric acid (80mL) . The solution was held at 70C for 24 hours under nitrogen.

Obtained HNMR but sulfuric acid was the main peak. Need C13 NMR but concentration is too low. Spinner on 300MHz NMR is not operating correctly. Sulfuric solution was diluted with 400mL of water. 2 x 150mL was taken out and one separated with methylene chloride and the other with benzene. TLC of the methylene chloride extraction revealed nothing as well as the benzene extraction.
2hr Video 10hr video 24hr video

No further tests have been done. Nothing else to report at this time.

9:30) t=0 sample taken, rheostat set at 51, starting temperature is 30C, solution is light brown
10:57) t=1hr 40min sample taken, temp from rheostat=51 is 61C, rheostat increased to 57, hood sash is fully open, solution is brown
11:18) temperature at 68C from rheostat=57, rheostat pushed to 59
12:15) temperature at 75C from rheostat=59, lowered rheostat to 55, solution is dark brown
15:10) temp=64 from rheostat=55, reset the rheostat set between 56-57, very dark solution, sample t=5.5 hrs
20:10) t=10.5hr sample taken, color same, temp=75C and hood sash was lowered and temp decreased to 68C, rheostat set to approx. 56

8:15) no change in color, sash remained at lowered position all night, rheostat at 56 and temperture at 72C


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