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10th July 2012 @ 03:29
MNR40-1%20scheme.png
mnr40-2%20table.PNG

Hazard and Risk Assessment:
HIRAC MNR37.pdf


Procedure:
A mixture of recovered SM from MNR40-1 (3.29 g, 10.74 mmol) and sulfur (0.69 g, 21.48 mmol) under argon was heated at 190°C in a sand bath for 2 hours.
Attached Files
3rd July 2012 @ 03:58
MNR40-1%20scheme.png
mnr40-1%20table.PNG

Hazard and Risk Assessment:
HIRAC MNR37.pdf


Procedure:
A mixture of MNR14-5 (3.9 g, 12.73 mmol) and sulfur (0.82 g, 25.46 mmol) under argon was heated at 190°C for 15 minutes by use of a heat gun. The mixture was then allowed to cool and diluted with EtOAc (20 mL) at which time a lot of solid crashed out of the mixture. Toluene (20 mL) was added and the mixture was heated to get everything into solution. The mixture was then left to cool and stand at room temperature. After 2 hours crystals had formed and they were filtered and washed with toluene. to give off white crystals 0.76 g - before washing there appeared to be more crystals so it can be assumed that a different solvent should be used to wash the crystals. The filtrate was concentrated to about 20 mL and left to stand overnight, more crystals appeared but they didn't look as clean. They were filtered and washed with toluene:hexane (50:50) to give what looked like a mixture of the above crystals and a yellow/orange solid.

1H NMR of the crystals showed that both drops were clean starting material

mnr40-1_1st crop.pdf


TLC (100% EtOAc) showed some reaction had occurred. spots from left to right. SM, Co, Crystals, Co, Filtrate. Product expected to run higher than SM.

SANY0202.JPG


1st crop 0.760 g
2nd crop 2.559 g

Total recovered by crystallisation 3.319 g
Attached Files