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31st October 2011 @ 04:32
Step 2 of 3 towards (S)-1,1'-binaphthyl-2,2'-disulfonic acid as for MW45-2

MNR18-1%20scheme.png

MNR18-1%20table.PNG

Hazard and Risk Assessment:
As for HIRAC-MNR17

Procedure
MNR16-1 (610 mg, 1.32 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 - 0.240 g - NOT PRODUCT

1H NMR MNR18-1

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.
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Attached Files
MNR18-1 scheme.png
MNR18-1 table.PNG
mnr18-1.pdf