反应 #2138435
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05099021
反应条件: temp:205.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 3.35 g (0.038 mol) of N,N-dimethylurea and 4.3 g (0.025 mol) of 4-bromoaniline were added with stirring into 28 ml of 1,2,4-trichlorobenzene, after which the mixture was slowly heated to 205° C. Dimethylamine was introduced from 50° C. After 5.5 hours, 11.6 g (0.25 mol) of dimethylamine had been introduced, and the reaction was complete. The reaction mixture was cooled to room temperature whereupon a precipitate deposited, which was filtered off, washed with 1,2,4-trichlorobenzene, dried at 100° C. in vacuo and then boiled in 100 ml of water. The aqueous mixture was cooled, and the precipitate was filtered off with suction and dried. 4.73 g of N-(4-bromophenyl)-N',N'-dimethylurea, i.e. 78% of theory, having a melting point of 168° to 170° C. were obtained in this way. The reaction mixture was cooled to room temperature whereupon a precipitate which was filtered off washed with 1,2,4-trichlorobenzene dried at 100° C. in vacuo The aqueous mixture was cooled the precipitate was filtered off with suction dried were obtained in this way
来源 ID: ord-c38bc2fa80a24675a8005dafcc542420