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20th March 2012 @ 03:34
MNR21-3%20scheme.png

mnr21-3%20table.PNG

DOI: 10.1002/chem.201002046

Hazard and Risk Assessment:
HIRAC MNR23-3.pdf


Water (60 mL) was added to a 500 mL round-bottomed flask. Sodium hydroxide (60.0 g, 1.5 mol) was added portionwise followed by a mixture of 2-phenylethylamine (24.3 mL, 0.19 mol), chloroform (16.0 mL, 0.19 mol), and benzyltriethylammonium chloride (400 mg, 1.8 mmol) in dichloromethane (60 mL)dropwise over 10 mins. The reaction mixture was then refluxed for 4 hours.

The reaction mixture was then allowed to cool to room temperature and was diluted with ice and water (50 mL), the organic layer was separated and retained, the aqueous layer was extracted with DCM (2 x 50 mL). The organic fractions were then combined and washed with HCl (1M) (3 x 100 mL) and brine (100 mL), dried over anhydrous magnesium sulfate, filtered and concentrated to give the crude as a dark orange oil (26.82 g) The crude was passed through a short column (60-100 EtOAC) collecting the top running spot. After concentration, (2-isocyanoethyl)benzene (MNR21-3) was afforded as a dark yellow oil (16.14 g, 64%)

1H NMR showed some EtOAC but other than that it was clean product

mn21-3_frac1.pdf


Product taken onto the next step
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Attached Files
MNR21-3 scheme.png
mnr21-3 table.PNG
HIRAC MNR23-3.pdf
mn21-3_frac1.pdf