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25th May 2012 @ 03:16
Repeat of MNR35-1 using only recrystalised starting material (MNR34-1)

Preparation of MNR35-1 - Step 2 in the alternative route to MNR26
Preparation of MNR34-1 - Step 1 in the alternative route to MNR26

MNR35-1%20scheme.png

mnr35-2%20table.PNG

Hazard and Risk Assessment:
MNR35

Procedure

To a solution of MNR34-1 (0.048 g, 0.19 mmol) in toluene (2 ml) was added 2,2-Diethoxyethylamine (0.05 mL, 0.37 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.

Monday: Column 0-10% MeOH/EtoAC+0.1%TEA

Frac 25-39 - 0.061 g, 0.17 mmol, 92%

mnr35-2_frac26-39.pdf
mnr35-2_frac26-39_13C.pdf
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Attached Files
mnr35-2 table.PNG
mnr35-2_frac26-39.pdf
mnr35-2_frac26-39_13C.pdf