Bromoacetone → HCID 86713417, Verbindung

HRID 64409

Reaktionsgleichung

[NH2:1][C:2]1[C:11]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[F:20])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=1.Br[CH2:22][C:23](=O)[CH3:24].C(=O)([O-])O.[Na+]>C(O)C>[F:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][O:12][C:11]1[C:2]2[N:3]([CH:22]=[C:23]([CH3:24])[N:1]=2)[CH:4]=[C:5]([C:6]([O:8][CH3:9])=[O:7])[CH:10]=1

Komponenten

Reaktionsbedingungen

Temperatur: 80 °C

Versuchsvorschrift

To a suspension of 2.15 g of methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate in 43 ml of ethanol was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, and the solvent was evaporated under reduced pressure, followed by extracting with ethyl acetate and washing with saturated brine. After drying over anhydrous magnesium sulfate and then filtering, the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 1.39 g of methyl 8-[(2-fluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-6-carboxylate.

Aufarbeitung

stirringby stirring at 80° C. for 4 hours
customthe solvent was evaporated under reduced pressure
extractionby extracting with ethyl acetate
washwashing with saturated brine
dry with materialAfter drying over anhydrous magnesium sulfate
filtrationfiltering
customthe solvent was evaporated under reduced pressure
customThe obtained residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag: ord-2d92678427e44e14afb990b87d1e5427
Quelldatensatz: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09447090B2

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