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Repeat of MNR35-2 on a 900 mg scale
Repeat Preparation of MNR35-2 - Step 2 in the alternative route to MNR26
Hazard and Risk Assessment:
MNR35
Procedure
To a solution of MNR34-2 (0.900 g, 3.49 mmol) in toluene (35 ml) was added 2,2-Diethoxyethylamine (0.86 mL, 6.98 mmol), and the mixture was heated to reflux for 2 hours during which time the reaction mixture turned from clear to yellow. The reaction was then allowed to cool to room temperature then cooled in an icebath. Again, as before, nothing crashed out so the mixture was concentrated and left in the freezer over the weekend.
Column 0-10% MeOH/EtOAc+0.1%TEA
Repeat Preparation of MNR35-2 - Step 2 in the alternative route to MNR26
Hazard and Risk Assessment:
MNR35
Procedure
To a solution of MNR34-2 (0.900 g, 3.49 mmol) in toluene (35 ml) was added 2,2-Diethoxyethylamine (0.86 mL, 6.98 mmol), and the mixture was heated to reflux for 2 hours during which time the reaction mixture turned from clear to yellow. The reaction was then allowed to cool to room temperature then cooled in an icebath. Again, as before, nothing crashed out so the mixture was concentrated and left in the freezer over the weekend.
Column 0-10% MeOH/EtOAc+0.1%TEA