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27th September 2011 @ 02:03
[b]Hazard and Risk Assessment:[/b] As for [url=http://www.ourexperiment.org/racemic_pzq/2339/Preparation_of_the_dimethoxy_Ugiintermediate_using_22Diethoxyethylamine.html]MNR8-1[/url] [b]Procedure[/b] To a mixture of formaldehyde solution (1.11 ml, 12.55 mmol), 2,2-dimethoxyethylamine (1.82 mL, 12.55 mmol) and cyclohexanecarboxylic acid (1.56 mL, 12.55 mmol) in methanol (10 mL) was added slowly 2-(3,4-Dimethoxyphenyl)ethyl isocyanide MNR4-1 (2.4 g, 12.55 mmol) and stirred at room temperature for 24 h. EtOAc (20 mL) was then added to the reaction and was washed with 1 M HCl (20 mL), sat. NaCO3 solution (20mL) and brine (20 mL), dried over MgSO4, filtered and concentrated. Crude:- 4.994 g as a dark orange oil FCC 2.882 g, 6.20 mmol, 49 % as a clear oil - why such a low yiels and low recovery from the column?? 1H NMR MNR8-2 similar to MNR8-1 [i]Lab book page complete, MNR[/i]
Attached Files
MNR8-2 scheme.png
MNR8-2 table.PNG
mnr08-2.zip
mnr8-2.pdf
mnr8-2_1H_500.pdf
mnr8-2_13C_500.pdf