Ammonium Chloride → HCID 20079668, Verbindung

Temperatur

60 °C

To a mixed solution of methyl 5-(difluoromethyl)thiophene-2-carboxylate (2.23 g) in tetrahydrofuran (60 ml) and methanol (15 ml) was added sodium borohydride (2.2 g) at room temperature, and the mixture was stirred at 60° C. for 1 hr. The reaction mixture was cooled to room temperature, saturated aqueous ammonium chloride solution was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (1.94 g).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)

ORD-Eintrag

ord-55ea9f3c517041628620183d3a26ebe3

Quelldatensatz

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09199963B2