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24th November 2011 @ 01:08
Further attempts to sort out the problems of the Newman-Kwart Rearrangement

Continuing on from MNR20-1 - MNR20-6

MNR20-1%20scheme.png

MNR20-1%20table.PNG

Hazard and Risk Assessment:
As for HIRAC-MNR17

Procedure
MNR20-7

MNR19-1 (70 mg, 0.15 mmol) in a sealed tube round was placed in a pre heated sand bath at 240-250°C (Heidolph hot plate). After 1 hour the tube was removed from the heat and allowed to reach room temperature.

Crude 1H NMR showed conversion but not complete or clean.

**NMR is named 20-6 but is actually 20-7**

25-75% EtOAC/Hex.

Product came out as very weak spots in fracs 15-23 - 15 mgs

1H NMR mnr20-7 frac 15-23

repeat above conditions with slightly longer reaction time.

Column, 5/12/11

Lab book page complete, MNR

Procedure
MNR20-8

MNR19-1 (40 mg, 0.09 mmol) in a sealed tube round was placed in a pre heated sand bath at 240-250°C (Heidolph hot plate). After 2 hours the tube was removed from the heat and allowed to reach room temperature.

Column:- 25-75% EtoAC/Hex

Frac 10-23
frac10-23

Frac 41-57 - mass?
product 12H peak resolves better at 500MHz

Lab book page complete, MNR
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Attached Files
mnr20-6_crude.pdf
mnr20-7_frac15-23.pdf
mnr20-8_frac10-25.pdf
mnr20-8_frac41-57.pdf
mnr20-7_frac15-23.zip
mnr20-8-f10-25.zip
mnr20-8-f41-57.zip