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22nd May 2012 @ 06:28
With requiring more MNR26 for resolutions, it's been decide to try the alternative route to MNR26 as the last attempt to scale up MNR11 has gone wrong with time and synthesised starting materials being wasted.

Meunier Eur. J. Org. Chem. 2008, 895–913
Zhou, Arch. Pharm. Chem. Life Sci. 2010, 343, 360 – 366

alt%20to%20mnr26.png

MNR34-1%20scheme.png

mnr34-1%20table.PNG


Hazard and Risk Assessment:
MNR34

Procedure

3,4-dimethoxyphenethylamine (6.42 mL, 38.6 mmol) and NaHCO3 (3.25 g, 38.6 mmol) were dissolved in DCM (50 mL) at room temperature. The mixture was cooled to 0 °C and chloroacetyl chloride (3.69 mL, 5.24 mmol) was added dropwise. The reaction mixture was stirred at 0 °C for 2 hours. Water (50 mL) was slowly added and the aqueous phase was extracted with DCM(100 mL). The organic layers were combined, washed with an aqueous solution of HCl (2M , 50 mL), dried with MgSO4, filtered, concentrated, and dried under vacuum. The crude off white solid was obtained (9.246 g) and was recrystalised with EtOH. The white crystals were washed with diethyl ether to give fine white crystals.

1st crop - fine white crystals 0.934 g

mnr34-1_first.pdf
mnr34-1_first_13C.pdf


2nd crop - fine white crystals 2.5 g

mnr34-1_second.pdf


left over - off white solid 4.769 g

mnr34-1_crude_after2.pdf


All fractions are as clean as each other therefore can take everything onto the next step.

Total recovered - 8.203, 82 %

** Experiment complete and closed **
Linked Posts
Attached Files
HIRAC MNR34.pdf
mnr34-1 table.PNG
alt to mnr26.png
MNR34-1 scheme.png
mnr34-1_crude_after2.pdf
mnr34-1_first.pdf
mnr34-1_first_13C.pdf
mnr34-1_second.pdf