Acetic Acid → Ethyl 3-(4-chloroanilino)but-2-enoate
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- customThe mixture was evaporated
- filtrationfiltered
- concentrationThe filtrate was concentrated
- customthe residue purified via column chromatography on silica gel with dichloromethane/hexane 4:1
출처 및 근거
- ORD 기록
- ord-25f4e5947d4f4c47a184d35ec991489a
- 출처 데이터셋
- uspto-grants-2002_06
- 특허 번호
- US06410562B1
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