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22nd March 2012 @ 05:45

Hazard and Risk Assessment:

As for MNR8-1

Procedure:

To a stirring suspension of paraformaldehyde (3.42 g, 114 mmol), 2,2-diethoxyethylamine (16.6 mL, 114 mmol) and cyclohexanecarboxylic acid (14.19 mL, 114 mmol) in methanol (65 mL) at 0 °C was added MNR21-3 (15.0 g, 114 mmol) in methanol (10 ml) dropwise and stirred at room temperature for XX hours.

The reaction was concentrated and dissolved in Et2O (150 mL) then washed with water (100 mL) and brine (100 mL) then dried over magnesium sulfate, filtered and concentrated under reduced pressure to give the crude as a dark brown oil, 53.795 g

Column #1 40-70% EtOAC/Hex (approx 500 ml silica, 500 ml fractions)

Frac 2-3 14.991 g 

mnr32-1_col1_frac2-3.pdf

Frac 4-5 14.825 g 

mnr32-1_col1_frac4-5.pdf

Frac 6-11 29.258 g 

mnr32-1_col1_frac6-11.pdf

Frac 12-13 0.105 g 

mnr32-1_col1_frac12-13.pdf

Total recovered - 59.179 g - 110%, thick oil is holding onto solvent, samples could be left on the high vac longer but they need re-columned.

All fraction need another column but this has got the quantities down to more manageable sizes.

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Attached Files
MNR32-1 scheme.png
mnr32-1 table.PNG
mnr32-1_col1_frac2-3.pdf
mnr32-1_col1_frac12-13.pdf
mnr32-1_col1_frac4-5.pdf
mnr32-1_col1_frac6-11.pdf