N,N'-Dimethylurea → 2-amino-4-fluoro-N-methylbenzamide
反応式
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].[CH3:12][NH:13]C(NC)=O>O>[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH:13][CH3:12])=[O:5]参加物
4
反応条件
- 温度
- 150 °C
実験手順
A mixture of 2-amino 4-fluoro benzoic acid (2.5 g, 16.13 mmol) and 1,3 dimethyl urea (5.85 g, 66.5 mmol) was heated at 150° C. for 24 hours. The reaction was diluted with water, filtered and extracted twice with ethyl acetate. The organic extracts were dried over magnesium sulfate and concentrated at reduced pressure. Chromatography on silica gel with ethyl acetate in hexanes (0-50%) gave the title compound as a waxy solid (670 mg, 25%)
後処理
- filtrationfiltered
- extractionextracted twice with ethyl acetate
- dry with materialThe organic extracts were dried over magnesium sulfate
- concentrationconcentrated at reduced pressure
出典と根拠
- ORDレコード
- ord-98808f368c2d4988b537d19cf74e01c2
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07875715B2
反応ノート
読み込み中…