All Notebooks | Help | Support | About
5th December 2011 @ 02:50
After column chromatography, MNR21-1 does not look clean and has what looks like intermediate N-phenethylformamide present. Is it possible to drive this to pure MNR21 with addition of more POCL3?


Hazard and Risk Assessment:

MNR21-1 (0.380 g, <2.56 ) and triethylamine (1.07 mL, 7.67 mmol) (was dissolved in dry DCM (5 mL) and phosphoryl chloride (0.25 mL, 2.56 mmol) was added dropwise added at 0°C. The mixture was then stirred for 1 h at 0°C and a further 4 h at room temperature. The mixture was quenched with water and neutralized with NaHCO3 solution. The organic layer was separated and the aqueous solution was extracted DCM (x3). The organic layers were combined, dried over magnesium sulphate, filtered and evaporated afforded a dark brown oil.

Crude NMR showed very little change from starting material. Reaction not taken forward. Alternative route attempted, see KAB4-1

Preparation of (2-isocyanoethyl)benzene (KAB4-1)

Lab book page complete, MNR
Linked Posts
This post is linked by:
Attached Files
MNR21-2 scheme.cdx
MNR21-2 scheme.png