反応式
[C:1]([C:3](=[CH:7][C:8]1[CH:13]=[C:12]([O:14][CH3:15])[C:11]([O:16][CH3:17])=[CH:10][C:9]=1[N+:18]([O-])=O)[C:4]([NH2:6])=[O:5])#[N:2]>[Fe]>[CH3:15][O:14][C:12]1[CH:13]=[C:8]2[C:9](=[CH:10][C:11]=1[O:16][CH3:17])[N:18]=[C:1]([NH2:2])[C:3]([C:4]([NH2:6])=[O:5])=[CH:7]2参加物
反応条件
- 温度
- 90 °C
実験手順
Iron powder (65.2 g., 1.22 moles) is added over a period of 1/2 hour to a slurry of α-cyano-β-(2-nitro-4,5-dimethoxyphenyl)acrylamide (75.0 g., 0.271 mole) in a 50% solution of acetic acid-N,N-dimethylgformamide (750 ml.) at 75° C. When addition of the iron powder is complete, the mixture is heated to 90° C. for 4 hours and then filtered while hot. The filter cake is washed with hot acetic acid (150 ml.). The dark red filtrate is gradually added to IN hydrochloric acid (1500 ml.) and the pink precipitate recovered by filtration and recrystallized from an excess (10%) of aqueous sodium hydroxide. The solid is filtered, washed with cold isopropanol and dried to give the title product as yellow crystals. Yield = 57.1 g. (83.5%); mpp. 274°-275° C.
後処理
- filtrationfiltered while hot
- washThe filter cake is washed with hot acetic acid (150 ml.)
- additionThe dark red filtrate is gradually added to IN hydrochloric acid (1500 ml.)
- filtrationthe pink precipitate recovered by filtration
- customrecrystallized from an excess (10%) of aqueous sodium hydroxide
- filtrationThe solid is filtered
- washwashed with cold isopropanol
- customdried
出典と根拠
- ORDレコード
- ord-85404ea15c7045678b5e4bed98078003
- 出典データセット
- uspto-grants-1978_10
- 特許番号
- US04120962
関連ノート
読み込み中…