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29th May 2012 @ 03:00
Preparation of MNR34-1 - Step 1 in the alternative route to MNR26

MNR34-1%20scheme.png

mnr34-2%20table.PNG

Hazard and Risk Assessment:
MNR34

Procedure

3,4-dimethoxyphenethylamine (8 mL, 48.17 mmol) and NaHCO3 (4.05 g, 48.17 mmol) were dissolved in DCM (60 mL) at room temperature under argon. The mixture was cooled to 0 °C and chloroacetyl chloride (4.05 mL, 48.17 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 and was recrystalised with EtOH/Hexane. The white crystals were washed with hexane to give fine white crystals.

1st crop 6.352 g, 24.65 mmol, 51 % as fine white crystals

2nd crop 1.017 g, 3.95 mmol, 8 % as fine white crystals

1H NMR

mnr34-2_1st.zip
Attached Files
mnr34-2 table.PNG
mnr34-2_1st crop.pdf
mnr34-2_1st.zip