反应 #2830900
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04043992
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 15.1 g. of phenyl N-methylcarbamate, 9.3 g. of aniline and 5.4 g. of the tetraethylammonium salt of 2-hydroxy-5-nitro-pyridine are refluxed in 200 ml. of ethanol for 5 hours. The reaction solution is concentrated, and the residue is dissolved in 100 ml. of chloroform, washed successively with 50 ml. of 1N sodium carbonate, 50 ml. of 1N hydrochloric acid and 100 ml. of water, and dried. By concentrating to dryness and recrystallizing from 120 ml. of ethanol, crystals of N-methyl-N-phenylurea having a m.p. of 150° - 151° C. are obtained in 91% yield. The reaction solution is concentrated the residue is dissolved in 100 ml of chloroform, washed successively with 50 ml of water, and dried By concentrating to dryness recrystallizing from 120 ml
来源 ID: ord-7a119bb21ff54d1eb77d350e75b11833