Reaktionsgleichung
CN(C1C=CC=CN=1)C.[C:10](OC(OC(C)(C)C)=O)(OC(C)(C)C)=[O:11].[CH3:25][O:26][C:27]([C:29]1([NH2:35])[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1)=[O:28].C(N(CC)CC)C.[CH2:43]([OH:49])[C:44]1[O:48][CH:47]=[CH:46][CH:45]=1>C1(C)C=CC=CC=1>[CH3:25][O:26][C:27]([C:29]1([NH:35][C:10]([O:49][CH2:43][C:44]2[O:48][CH:47]=[CH:46][CH:45]=2)=[O:11])[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34]1)=[O:28]Komponenten
Edukt 5
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3.67 g (30 mmol) of dimethylaminopyridine was added to a solution of 65.48 g (0.3 mol) of di-t-butyl dicarbonate in 300 ml of anhydrous toluene, and the mixture was stirred at room temperature for 15 minutes. A solution of 47.17 g (0.3 mol) of 1-aminocyclohexanecarboxylic acid methyl ester in 100 ml of anhydrous toluene was added to the reaction solution, and the mixture was stirred at room temperature for 1 hour. Further, after 60.71 g (0.6 mol) of triethylamine and 44.1 g (0.45 mol) of furfuryl alcohol were added, the mixture was heated under reflux for 3 hours. The reaction solution was returned to room temperature and was concentrated under reduced pressure. The obtained residue was crushed by a mortar and stirred in a mixture solution of 5 ml of hydrochloric acid and 3 L of water for 18 hours. The obtained crystal was collected by filtration to obtain 74.37 g (88%) of the title compound.
Aufarbeitung
- stirringthe mixture was stirred at room temperature for 1 hour
- temperaturethe mixture was heated
- temperatureunder reflux for 3 hours
- customwas returned to room temperature
- concentrationwas concentrated under reduced pressure
- customThe obtained residue was crushed by a mortar
- stirringstirred in a mixture solution of 5 ml of hydrochloric acid and 3 L of water for 18 hours
- filtrationThe obtained crystal was collected by filtration
Quellen und Nachweise
- ORD-Eintrag
- ord-5928be8d50334571bd5c8ddf93fcf419
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08829209B2
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