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29th May 2012 @ 03:04
MNR36-1%20scheme.png

mnr36-1%20table.PNG

Hazard and Risk Assessment:
MNR34

Procedure

2-phenethylamine (7.0 mL, 55.57 mmol) and NaHCO3 (4.67 g, 55.57 mmol) were dissolved in DCM (70 mL) at room temperature under argon. The mixture was cooled to 0 °C and chloroacetyl chloride (5.30 mL, 66.68 mmol) was added dropwise - Upon addition a white precipitate formed and the reaction stopped stirring, DCM (40 mL) was added to free up this solid and to allow stirring to continue. The reaction mixture was stirred at 0 °C for 3 hours. Water (50 mL) was slowly added and the aqueous phase was extracted with DCM (100 mL). The organic layers were combined, washed with HCl (2M , 50 mL), dried with MgSO4, filtered, concentrated, and dried under vacuum to give grey/off white crystals. The crude was recrystallised with EtOH/hexane and washed with hexane to give fine off white crystals.

1st crop 4.515 g, 22.8 mmol, 41 % as off white crystals

2nd crop 2.590 g, 13.1 mmol, 24 %

1H NMR
13C NMR

mnr36-1_1st.zip
Attached Files
mnr36-1 table.PNG
MNR36-1 scheme.png
mnr36-1_1st.zip
mnr36-1_1st crop.pdf
mnr36-1_1st crop_13C.pdf