Acetic Acid → Ethyl 3-(4-chloroanilino)but-2-enoate
反応式
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[C:9]([O:15][CH2:16][CH3:17])(=[O:14])[CH2:10][C:11]([CH3:13])=O.C(O)(=O)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][C:11]([CH3:13])=[CH:10][C:9]([O:15][CH2:16][CH3:17])=[O:14])=[CH:4][CH:3]=1参加物
5
実験手順
A solution of 70 g (0.54 mol) of 4-chloroaniline, 70 ml (0.54 mol) of ethyl acetoacetate, and 0.6 ml acetic acid in 400 ml toluene was heated in a Dean-Stark apparatus for 19 at 130° C. The mixture was evaporated, and the remaining crystalline precipitate stirred with diisopropylether and filtered. The filtrate was concentrated and the residue purified via column chromatography on silica gel with dichloromethane/hexane 4:1.
後処理
- customThe mixture was evaporated
- filtrationfiltered
- concentrationThe filtrate was concentrated
- customthe residue purified via column chromatography on silica gel with dichloromethane/hexane 4:1
出典と根拠
- ORDレコード
- ord-25f4e5947d4f4c47a184d35ec991489a
- 出典データセット
- uspto-grants-2002_06
- 特許番号
- US06410562B1
反応ノート
読み込み中…