(1-Chloroethyl)carbamyl chloride → Vinyl isocyanate

Participants

Reaction Steps

563 parts of 1-chloroethylcarbamyl chloride are dissolved in 2,800 parts by volume of hexamethylene diisocyanate. The solution, totalling 3,100 parts by volume, is introduced in 3 portions (500, 1,500 and 1,100 parts by volume) with different residence times (150, 310 and 225 minutes respectively) into a thin film evaporator operated under atmospheric pressure, with a counter-current of nitrogen. The jacket temperature is 73°-75° C. and the material passes over at 48°-54° C. The reaction product is collected in a receiver and two downstream cold traps, and the composition is determined by gas chromatography. 145.3 parts (53% of theory) of vinyl isocyanate, of boiling point 38.5° C./1,013 mbar, and 73.8 parts (17.7% of theory) of 1-chloroethyl isocyanate, of boiling point 92° C./1,013 mbar, are obtained.

Provenance & Evidence