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2nd November 2012 @ 22:26
Mnr: MNR51-60
EDC Coupling of MNR51 with methylamine to give MNR53-1

See - Synthesis of AEW16-1
- Synthesis of MNR52-1



MNR53-1_table.PNG

Hazard Assessment
HIRAC MNR53.pdf


Procedure

reaction on at 430pm 6/11/12

EDCI (0.111 g, 0.48 mmol) and HOBt (0.007 g, 0.05 mmol) were added to a solution of MNR51-2 (0.140 g, 0.48 mmol) in DCM (7 mL) and the mixture was stirred for 20 minutes. Methylamine in water (35%, 0.5 mL) was added and the reaction mixture stirred at room temperature. After stirring overnight the TLC showed spot to spot conversion. The reaction was quenched with sodium bicarbonate (10 mL) and extracted with with DCM (3 x 10 mL), dried over MgSO4, filtered and concentrated to give a brown oil (0.147 g).

TLC 100% EtOAc
MNR53-1_rxn.JPG


short column, 75-100% EtOAc/Hex

fracs 29-46 0.054 g, as a clear oil which slowly crystallised to give white crystals. 1H NMR showed large water peak. Unsure where this has come from

NMR

mnr53-1_frac29-49_1H.pdf


mnr53-1_conc_1H.pdf

mnr53-1_conc_13C.pdf
mnr53-1_conc_19F.pdf
mnr53-1_conc.zip
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Attached Files
MNR53_scheme.png
MNR53-1_table.PNG
MNR53-1_table.PNG
HIRAC MNR53.pdf
MNR53-1_rxn.JPG
mnr53-1_frac29-49_1H.pdf
mnr53-1_conc.zip
mnr53-1_conc_1H.pdf
mnr53-1_conc_13C.pdf
mnr53-1_conc_19F.pdf
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