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21st November 2011 @ 03:21

Preparation of (2-isocyanoethyl)benzene (MNR21-1)

Hazard and Risk Assessment:

Procedure: To a mixture of formaldehyde solution (0.30 ml, 3.35 mmol), 2,2-dimethoxyethylamine (0.49 mL, 3.35 mmol) and benzoic acid (0.41 g, 3.35 mmol) in methanol (1 mL) was added slowly 2-(3,4-Dimethoxyphenyl)ethyl isocyanide MNR21-1(0.44 g, 3.35 mmol)in MeOH (1.5 mL) 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.

*Note:- If formation of desired starting material had not gone to completetion in the previuos step then it's not expected to get a good return if any from this reaction.

 

1H NMR 

mnr22-1_frac10-16.pdf

Lab book page complete, MNR

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Attached Files
MNR22-1 scheme.png
mnr22-1 table.PNG
mn21-1_2nd col.pdf
mnr22-1_col1_topspot.zip
mnr22-1_frac4-7.zip
mnr22-1_frac10-16.zip
mnr22-1_frac10-16.pdf