Tetraethylammonium → N-Methyl-N-phenylurea
反応式
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]参加物
6
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-fa3c2551b7d24fc7b8b133895d4d4b40
- 出典データセット
- uspto-grants-1976_06
- 特許番号
- US03963728
反応ノート
読み込み中…