Tetraethylammonium → N-Methyl-N-phenylurea
반응식
CNC(=O)O[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[NH2:12]C1C=CC=CC=1.C([N+](CC)(CC)CC)C.[OH:28][C:29]1C=CC([N+]([O-])=O)=[CH:31][N:30]=1>C(O)C>[CH3:31][N:30]([C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1)[C:29]([NH2:12])=[O:28]참가 물질
6
실험 절차
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.
후처리
- concentrationThe reaction solution is concentrated
- dissolutionthe residue is dissolved in 100 ml
- washof chloroform, washed successively with 50 ml
- dry with materialof water, and dried
- concentrationBy concentrating to dryness
- customrecrystallizing from 120 ml
출처 및 근거
- ORD 기록
- ord-fa3c2551b7d24fc7b8b133895d4d4b40
- 출처 데이터셋
- uspto-grants-1976_06
- 특허 번호
- US03963728
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