Potassium Carbonate → 2-[2-Chloro-4-(1-pyrazolyl)methylphenoxy]ethylcarbamic acid methyl ester
Reaktionsgleichung
[C:1](=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:13]=[C:12]([CH2:14][N:15]2[N:19]=[CH:18][CH:17]=N2)[CH:11]=[CH:10][C:9]=1[OH:20].[CH3:21][O:22][C:23](=[O:28])[NH:24][CH2:25][CH2:26]Cl.[Cl-].[NH4+]>CN(C)C=O>[CH3:21][O:22][C:23](=[O:28])[NH:24][CH2:25][CH2:26][O:20][C:9]1[CH:10]=[CH:11][C:12]([CH2:14][N:15]2[CH:1]=[CH:17][CH:18]=[N:19]2)=[CH:13][C:8]=1[Cl:7]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
To a mixture of potassium carbonate (435 mg), 2-chloro-4-(2-2H-1,2,3-tri-azolyl)methylphenol (300 mg) and anhydrous N,N-dimethylformamide (30 ml) was added dropwise an anhydrous N,N-dimethylformamide solution (2 ml) of 2-chloroethylcarbamic acid methyl ester (216 mg) at room temperature under stirring. This mixture was then heated at 60° C. under stirring for 6 hours, and poured into ice-cooled saturated aqueous ammonium chloride solution, which was extracted with ethyl acetate. The organic layer was washed with water and then saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, which afforded 329 mg of 2-[2-chloro-4-(1-pyrazolyl)methylphenoxy]ethylcarbamic acid methyl ester (compound 7). Yield, 74%.
Aufarbeitung
- stirringunder stirring for 6 hours
- additionpoured into ice-
- extractionwas extracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialsaturated sodium chloride solution, dried with anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-7fb194e164834ab09957857f7bedc501
- Quelldatensatz
- uspto-grants-1997_11
- Patentnummer
- US05684022
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