Reaktion #61776
ord-b69f2cc62b6e45c99bba0ce84dda59b6
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.STIRRINGstirring
- 2Sonstigecontinued at room temperature
- 3Sonstige(r.t.) overnight
- 4workup.STIRRINGwas stirred for 1 h
- 5Sonstigethe formed precipitate isolated by filtration
- 6Waschenwashed with water, water/methanol 1:1, n-heptane, and ether
- 7SonstigeThe residue was dried at 40° C. in vacuum
Vorschrift
29 mg (0.73 mmol) of 60% sodium hydride were added to at 0° C. to a solution of 152 mg (0.70 mmol) 4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 8.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 200 mg (0.70 mmol) 3-chloromethyl-2-methyl-6-(3-trifluoromethyl-phenyl)-pyridine (WO 2005/049573) were given to the reaction mixture and stirring continued at room temperature (r.t.) overnight. After addition of 16 ml water the mixture was stirred for 1 h, the formed precipitate isolated by filtration, washed with water, water/methanol 1:1, n-heptane, and ether. The residue was dried at 40° C. in vacuum to give 288 mg (88%) of the title compound as beige powder.