Ethyl isocyanate → HCID 68839047, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of the product of Step 1 (0.37 g, 1.21 mmol), ethylisocyanate (0.43 g, 6.05 mmol) and a catalytic quantity of dibutyltin diacetate (5 drops) in THF/toluene (1:1, 10 mL) was heated in a sealed tube at 100° C. for 15 h. This mixture was cooled to 0° C., the solid obtained was filtered and washed with 10% CHCl3/hexanes to isolate crude product. The solid was taken up into MeOH/CHCl3, and dried onto silica gel. This material was then purified by column chromatography on silica gel (1-8% MeOH/CHCl3 as eluant) followed by trituration with chloroform (10 mL) and hexanes (500 mL) to isolate the title compound as a solid. LCMS (APCI+) 377.

Provenance & Evidence