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UC on ChemSpider
Alicia's Masters Thesis
Open Web Drug Dev.
To Do List
Ugi NMR Analysis
To repeat the optimization reaction conducted in
to make this
using Mettler Toledo's automated Minimapper. Forty eight reactions are run in parallel using four reactant (2.0M in methanol) in different solvents / concentration.
Make up 2M methanol solutions (50mL each) of starting materials - Benzaldehyde (10.550mL), Furfurylamine (8.837mL), Boc-glycine (17.518g) and tert-butyl isocyanide (11.310mL).
The following are added in this order in a reaction tube equipped with a filtration frit
1) The additional solvent (200uL methanol)
2) The benzaldehyde solution
3) The Furfurylamine solution
4) The Boc-Glycine solution
5) The tert-butyl isocycanide solution
Parameters to modify:
concentration - 0.5M, 0.25M and 0.1M
reagent excess - 1.0 and 1.2 equivalents
solvent (for 0.25 and 0.1 conc only): ethanol, acetonitrile, THF
This is 48 experiments total and they are listed in this
The results are not meaningful because the liquid handler was not properly programmed.
log file 2
14:20 Moved the miniblock from the mapper to the shaker and started shaking (600rpm)
15:30 Removed the miniblock from the shaker and drained excess solvents..
16:00 Added methanol (1mL) to each reaction tube and set it on the shaker
16:20 Removed from the shaker, drained methanol, added more methanol (1mL) to each reaction tube again and set the miniblock on the shaker..
16:50 Removed from the shaker and drained out methanol...left the miniblock connected to vacuum.
13:00 Removed from vacuum and added dichloromethane (2mL) to each reaction tube in the miniblock.
13:30 Set the block again on the shaker.
17:00 Removed from the shaker and drained the solution of the product and dichloromethane in to collecting tubes, connected to vacuum, inorder to remove excess dichloromethane.
15:00 Removed from under the house vac and placed it in a desiccator connected to a vacuum pump in ordesr to dry off the solvent completely.
19:00 Obtained the weights of the sample tubes with the products.
InChI=1/C24H33N3O5/c1-23(2,3)26-21(29)20(17-11-8-7-9-12-17)27(16- 18-13-10-14-31-18)19(28)15-25-22(30)32-24(4,5)6/h7-14,20H,15-16H2 ,1-6H3,(H,25,30)(H,26,29)
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