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2nd May 2012 @ 23:59
MNR8-3%20scheme.png


Hazard and Risk Assessment:

As for MNR8-1

Procedure:

To a stirring suspension of paraformaldehyde (2.81 g, 93.60 mmol), 2,2-dimethoxyethylamine (13.61 mL, 93.6 mmol) and cyclohexanecarboxylic acid (11.61 mL, 93.6 mmol) in methanol (90 mL) at 0 °C was added 2-(3,4-Dimethoxyphenyl)ethyl isocyanide MNR4-2 (17.9 g, 93.6 mmol) dropwise and stirred at room temperature for 48 hours.

The reaction was concentrated and dissolved in EtOAc (75 mL) then washed with water (50 mL) and brine (50 mL) then dried over magnesium sulfate, filtered and concentrated under reduced pressure to give the crude as a pale yellow oil.

** Reagents were added in the wrong order and it looks like the reaction hasn't worked. After two columns in an attempt to recover isocyanide the following fractions were collected.

Column :- 40-80 % EtOAc/Hex

Frac 1-2 yellow oil 3.941 g
Frac 3-5 white solid 12.27 g
Frac 6-7 yellow solid 3.659 g