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30th May 2013 @ 05:59

Repeated to collect data for paper - see original experiment Reductive amination of pyrrole aldehyde with crude PMY 53-2 (PMY 56-1)


PMY 2-5 (91 mg, 0.42 mmol, 1 equiv.) and crude PMY 53-2 (37 mg, ~0.42 mmol) were dissolved in MeOH (5 mL) and acetic acid (0.13 mL) and stirred for 1 hour at room temperature. Sodium cyanoborohydride (37 mg, 1.01 mmol, 1.1 equiv.) was added. After 1 hour, no product was observed by TLC. Reaction mixture was stirred for 20 hours and no product spot observed by TLC.

Volatiles were removed in vacuo and then 1M NaOH added and the mixture extracted with CH2Cl2, organic layer washed with brine, dried (MgSO4), filtered and evaporated to give a pale brown oil.

Crude indicated desired product - Purified by flash column (1-15% MeOH) no product recovered.

 

Data:

AEW 60-1 crude.zip
Attached Files
AEW-60-1.png
AEW 60-1 crude.zip