Ethanol → HCID 178471868, compound
Reaction equation
[CH:1]1([NH2:4])[CH2:3][CH2:2]1.[Cl:5][C:6]1[CH:21]=[C:20]([Cl:22])[C:19]([F:23])=[CH:18][C:7]=1[C:8]([C:10](=[CH:14][O:15][CH2:16][CH3:17])[C:11]([O-])=O)=[O:9].C([OH:26])C>>[Cl:5][C:6]1[CH:21]=[C:20]([Cl:22])[C:19]([F:23])=[CH:18][C:7]=1[C:8]([C:10](=[CH:11][NH:4][CH:1]1[CH2:3][CH2:2]1)[C:14]([O:15][CH2:16][CH3:17])=[O:26])=[O:9]Participants
4
Procedure
4.5 g of cyclopropylamine are added dropwise to a solution of 24.9 g of ethyl(2-(2,4-dichloro-5-fluorobenzoyl)-3-ethoxy-acrylate in 80 ml of ethanol, while cooling with ice and stirring. When the exothermic reaction has subsided, stirring is continued at room temperature for 1 hour, the solvent is stripped off in vacuo and the residue is recrystallized from cyclohexane/petroleum ether. 22.9 g of ethyl 2-(2,4-dichloro-5-fluoro-benzoyl)-3-cyclopropylamino-acrylate of melting point 89°-90° C. are obtained.
Workup
- temperaturewhile cooling with ice
- customWhen the exothermic reaction
- stirringstirring
- customthe residue is recrystallized from cyclohexane/petroleum ether
Sources & evidence
- ORD record
- ord-6dd79a6391c049ed9fcb10efacb6c458
- Source dataset
- uspto-grants-1986_01
- Patent number
- US04563459
Reaction notes
Loading…