Reaktionsgleichung
ClC([O:4][CH2:5][CH3:6])=O.O[C:8]1[CH:9]=[C:10]([CH:16]=[CH:17][C:18]=1[O:19][CH3:20])[CH:11]=[CH:12][C:13]([OH:15])=O.C(N(CC)CC)C.[NH2:28][CH:29]1[CH2:36][CH2:35][CH2:34][NH:33][C:31](=[O:32])[CH2:30]1.C1C[O:40]CC1>>[CH2:5]([O:4][C:20]([O:19][C:18]1[CH:8]=[CH:9][C:10]([CH:11]=[CH:12][C:13]([NH:28][CH:29]2[CH2:36][CH2:35][CH2:34][NH:33][C:31](=[O:32])[CH2:30]2)=[O:15])=[CH:16][CH:17]=1)=[O:40])[CH3:6]Komponenten
Versuchsvorschrift
Ethyl chloroformate (22.2 ml) was added dropwise to a mixture of 3-hydroxy-4-methoxycinnamic acid (22.5 g), triethylamine (32.3 ml) and THF (400 ml) under ice-cooling and stirring, followed by stirring for 15 mins. Subsequently, to the mixture was added dropwise a solution of 3-amino-ε-caprolactam (14.9 g) in THF (200 ml), and then the whole was stirred for 1 hr. at room temperature. After completing the dropping, the reaction mixture was concentrated under reduced pressure, and the residue was dissolved in chloroform. This solution was washed with water, dried and distilled under reduced pressure to remove the solvent. The residue was washed with ethyl acetate, dried under reduced pressure to give the title compound (28 g). This compound was used in the following reaction without purification.
Aufarbeitung
- temperaturecooling
- stirringby stirring for 15 mins
- stirringthe whole was stirred for 1 hr
- customat room temperature
- concentrationwas concentrated under reduced pressure
- dissolutionthe residue was dissolved in chloroform
- washThis solution was washed with water
- customdried
- distillationdistilled under reduced pressure
- customto remove the solvent
- washThe residue was washed with ethyl acetate
- customdried under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-2f7299906dbe4a1e92167c16c3c5d7ce
- Quelldatensatz
- uspto-grants-1992_06
- Patentnummer
- US05118806
Verknüpfte Notizen
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