反应 #3703288
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04607044
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 16.0 g. of 2,6-dichlorobenzoylisocyanate are added in small portions to a solution of 11.66 g. of p-chloroanilino-acetonitrile in 100 ml. of dry benzene with moderate cooling. After some time a substance crystallizes out, which after about 12 hours is drawn off and washed with benzene. After drying the weight is 25.25 g, i.e. 93.7% the melting point being 185° C., with spontaneous decomposition on the Kofler heating bench. Thin-layer chromatography (solvent either ethylacetate or chloroform) shows that the substance is pure, however, if desired, it may be recrystallized from 250 ml. of benzene with a yield of 80%. After some time a substance crystallizes out washed with benzene After drying the weight being 185° C., with spontaneous decomposition on the Kofler heating bench it may be recrystallized from 250 ml
来源 ID: ord-7962ad37452f406b995ffe7e656a701f