反応式
[Cl:1][C:2]1[CH:14]=[C:13]([N+:15]([O-])=O)[CH:12]=[CH:11][C:3]=1[NH:4][C:5](=[O:10])[CH2:6][CH2:7][CH2:8][CH3:9]>C(O)(=O)C.[Fe]>[NH2:15][C:13]1[CH:12]=[CH:11][C:3]([NH:4][C:5](=[O:10])[CH2:6][CH2:7][CH2:8][CH3:9])=[C:2]([Cl:1])[CH:14]=1参加物
4
実験手順
2'-Chloro-4'nitrovaleranilide (13.0 g.) is dissolved in warm glacial acetic acid (100 ml.) and iron powder (14 g.) is added portionwise to maintain gentle boiling. The resulting reaction mixture is refluxed for one-half hour and filtered. The filtrate is evaporated under reduced pressure and the residue is triturated with water. The solid that forms is collected (11.5 g.) and recrystallized from cyclohexane to yield 7.5 g., m.p. 96.5°-99° C.
後処理
- temperatureto maintain gentle boiling
- customThe resulting reaction mixture
- temperatureis refluxed for one-half hour
- filtrationfiltered
- customThe filtrate is evaporated under reduced pressure
- customthe residue is triturated with water
- customThe solid that forms is collected (11.5 g.)
- customrecrystallized from cyclohexane
- customto yield 7.5 g
出典と根拠
- ORDレコード
- ord-e1f3fe92ed7446659ef309a2a51feb71
- 出典データセット
- uspto-grants-1977_02
- 特許番号
- US04006233
関連ノート
読み込み中…