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31st October 2011 @ 04:15
Step 2 of 3 towards (R)-1,1'-binaphthyl-2,2'-disulfonic acid as for MW45-2

MNR17-1%20scheme.png

MNR17-1%20table.PNG

Hazard and Risk Assessment:
HIRAC-MNR17

Procedure

MNR15-1 (680 mg, 1.48 mmol) was placed in a roundbottom flask (100 ml) and heated in a heating mantle to 250°C for 90 min. The dark brown solid was dissolved in chloroform and purified by column chromatography (silica gel, 5% EtoAC/Hex).

Major spot - 0.131 g - NOT PRODUCT

1H NMR MNR17-1

Not sure what's gone wrong here. The crude product was not totally soluble and was stuck to flask. Heated for too long or too hot? Hard to control the temperature of the mantle.
Attached Files
MNR17-1 table.PNG
MNR17-1 scheme.png
HIRAC MNR17.pdf
mnr17-1.pdf