Hydrochloric Acid → HCID 6713300, Verbindung
Reaktionsgleichung
Cl.[CH3:2][C:3]([CH3:9])([C:5](=[O:8])[CH2:6][CH3:7])[CH3:4].[N:10](OCCCC)=[O:11]>C(OCC)C.C1(C)C=CC=CC=1>[OH:11][N:10]=[C:6]([CH3:7])[C:5](=[O:8])[C:3]([CH3:9])([CH3:4])[CH3:2]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- -10 °C
Versuchsvorschrift
A solution of 40 g of hydrogen chloride in 156 g of diethyl ether is added dropwise at room temperature to 96 g (0.84 mol) of 2,2-dimethyl-3-pentanone in 960 g of toluene. After cooling to -10° C., a solution of 95 g of n-butyl nitrite in 470 g of diethyl ether is added dropwise. The mixture is stirred at from -10° C. to 0° C. for 4 hours and then allowed to come to room temperature. After a total of 16 h, the reaction mixture is washed three times with 1 l of ice-water each time and then extracted twice with 1 l of 1M sodium hydroxide solution each time. The alkaline phase is separated off and neutralized with 20% strength sulfuric acid. The crude product is filtered off with suction and, after drying, recrystallized from n-hexane. 66 g (55%) of the title compound are obtained as a pale yellow powder of melting point 107-110° C.
Aufarbeitung
- customto come to room temperature
- washAfter a total of 16 h, the reaction mixture is washed three times with 1 l of ice-water each time
- extractionextracted twice with 1 l of 1M sodium hydroxide solution each time
- customThe alkaline phase is separated off
- filtrationThe crude product is filtered off with suction
- customafter drying
- customrecrystallized from n-hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-791c0473cdd6424582399b685a7637c9
- Quelldatensatz
- uspto-grants-2000_10
- Patentnummer
- US06127568
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