反応式
[NH2:1]/[C:2](/[C:9]([F:12])([F:11])[F:10])=[CH:3]\[C:4]([O:6]CC)=O.N12CCCN=C1CCCCC2.[Cl:24][C:25]1[C:40]([CH3:41])=[C:39]([N+:42]([O-:44])=[O:43])[C:28]([NH:29][C:30](OC2C=CC=CC=2)=[O:31])=[C:27]([F:45])[CH:26]=1.Cl>CN(C)C=O.O>[Cl:24][C:25]1[CH:26]=[C:27]([F:45])[C:28]([N:29]2[C:4](=[O:6])[CH:3]=[C:2]([C:9]([F:10])([F:11])[F:12])[NH:1][C:30]2=[O:31])=[C:39]([N+:42]([O-:44])=[O:43])[C:40]=1[CH3:41]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- -10 °C
実験手順
Ethyl 3-amino-4,4,4-trifluorocrotonate (6.1 g, 33.1 mmol) was dissolved in dimethylformamide (47 ml) and stirred at −10 ° C. To this solution was slowly added 1,8-diazabicyclo[5.4.0]undec-7-ene (6.3 g, 41.4 mmol) and solution stirred for 0.5 hr. To this solution was slowly added a solution of 4-chloro-2-fluoro-5-methyl-6-nitro-N-phenoxycarbonylaniline (8.5 g) in dimethylformamide (25 ml) followed by stirring at ambient temperature for 14 hr. Solution was then heated to 80 ° C. and stirred at this temperature for 4 hr. Water was added and pH adjusted to 4 by addition of dilute hydrochloric acid. Product was extracted with ethyl acetate followed by evaporation of the solvent to afford the crude product (10.1 g) which was subjected to N-methylation as follows.
後処理
- stirringstirred for 0.5 hr
- stirringby stirring at ambient temperature for 14 hr
- temperatureSolution was then heated to 80 ° C.
- stirringstirred at this temperature for 4 hr
- extractionProduct was extracted with ethyl acetate
- customfollowed by evaporation of the solvent
出典と根拠
- ORDレコード
- ord-25819bacf4194d958d5590a297597818
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06355799B1
関連ノート
読み込み中…