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27th September 2011 @ 02:16
MNR10-1%20scheme.png

MNR10-1%20table.PNG

Hazard and Risk Assessment:
HIRAC MNR10.pdf


Procedure:

To a mixture of formaldehyde solution (1.94 ml, 21.96 mmol), 2,2-dimethoxyethylamine (3.19 mL, 21.96 mmol) and benzoic acid (2.68 g, 21.96 mmol) in methanol (15 mL) was added slowly 2-(3,4-Dimethoxyphenyl)ethyl isocyanide MNR4-1 (4.20 g, 21.96 mmol) and stirred at room temperature for 24 h. EtOAc (20 mL) was then added to the reaction and was washed with 1 M HCl (20 mL), sat. NaCO3 solution (20mL) and brine (20 mL), dried over MgSO4, filtered and concentrated.

Crude:- 9.48 g as a yellow/orange oil

Column:- 20-100% EtOAc/Hex

6.796 g as a thick clear oil

LCMS

LCMS MNR11-6
Ret. Time
18.8___481.3 [M+H]
_______413.3 [Hemiaminal+H]
_______497.2 Unknown
25.3___Impurities found in the MeoH used to make up samples.

Hemiaminal cyclisation happening in the mass spec?

1H NMR MNR10-1

Lab book page complete, MNR
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Attached Files
MNR10-1 table.PNG
MNR10-1 scheme.png
HIRAC MNR10.pdf
MNR10-1 scheme.png
LCMS_mnr10-1.pdf
LCMS_MeOH_blank.pdf
mnr10-1.pdf
mnr10-1.zip