(1-Chloroethyl)carbamyl chloride → Vinyl isocyanate

Participants

Reaction Steps

563 parts of 1-chloroethylcarbamic acid chloride are dissolved in 2,800 parts by volume of hexamethylene diisocyanate. The solution, having a total volume of 3,100 parts, 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 which is operated under atmospheric pressure, with a stream of nitrogen passing through in counter-current. The jacket temperature is 73°-75° C. and the material passes over at 48° to 54° C. The product is collected in a receiver and two downstream cold traps and the composition of the product is determined by gas chromatography. 145.3 parts (53% of theory) of vinyl isocyanate of boiling point 38.5° C./1013 mbar and 73.8 parts (17.7% of theory) of 1-chloroethyl isocyanate of boiling point 92° C./1013 mbar are obtained.

Provenance & Evidence