叔辛基异氰酸酯

反应条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A reaction vessel is charged with 100 parts of ethyl acetate, 17.7 parts of 3'-hydroxy-2-methylacrylanilide, 23.3 parts of 1,1,3,3-tetramethylbutyl isocyanate and 4 parts of triethylamine. The reaction mixture is heated at reflux for about 18 hours with stirring, and then 100 parts of benzene and 50 parts of hexane are added. The reaction mixture is cooled to -15°C and filtered. The solids are washed with hexane and recrystallized from aqueous alcohol to give 12.5 parts of 3'-(1,1,3,3-tetramethylbutylcarbamoyloxy)-2-methylacrylanilide, m.p. 118°-120°C. The reaction mixture is heated at reflux for about 18 hours filtered The solids are washed with hexane recrystallized from aqueous alcohol