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23rd March 2012 @ 04:10
MNR22-2%20scheme.png
mnr22-2%20table.PNG

Hazard and Risk Assessment:

As for MNR8-1

Procedure:

To a stirring suspension of paraformaldehyde (3.89 g, 130 mmol), 2,2-diethoxyethylamine (18,8 mL, 130 mmol) and benzoic acid (15.8 g, 114 mmol) in methanol (75 mL) at 0 °C was added MNR21-3 (17.0 g, 114 mmol) in methanol (10 ml) dropwise and stirred at room temperature over the weekend, 65 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, 43.88 g

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

Frac 2-3 12.856 g
Frac 4-7 27.500 g
Frac 8-10 1.775 g

Total recovered - 42.111 g

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

mnr22-2_col1_frac2-3.pdf
mnr22-2_col1_frac4-7.pdf
mnr22-2_col1_frac8-10.pdf
Attached Files
MNR22-2 scheme.png
mnr22-2 table.PNG
mnr22-2_col1_frac2-3.pdf
mnr22-2_col1_frac4-7.pdf
mnr22-2_col1_frac8-10.pdf