Potassium Carbonate → HCID 89995600, Verbindung

Temperatur

120 °C

(3-Hydroxy-4-nitrophenyl)(3-methoxyazetidin-1-yl)methanone (Preparation 115, 300 mg, 1.19 mmol) and methyl 2-chloro-2,2-difluoroacetate (258 mg, 1.78 mmol) were dissolved in dry DMF (2 mL). Potassium carbonate (328 mg, 2.38 mmol) was added and the reaction was heated to 120° C. under microwave irradiation for 1 hour. The reaction was cooled to room temperature and diluted with ethyl acetate (20 mL). The organic solution was washed with water (20 mL), brine (20 mL), dried over sodium sulphate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a gradient of 20% hexanes in ethyl acetate to 100% ethyl acetate to afford the title compound as a yellow oil (250 mg, 67.3%).

1. temperatureThe reaction was cooled to room temperature
2. washThe organic solution was washed with water (20 mL), brine (20 mL)
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by silica gel column chromatography
6. washeluting with a gradient of 20% hexanes in ethyl acetate to 100% ethyl acetate

ORD-Eintrag

ord-a0cb2ec27fb14f3fbfe6c250a6608699

Quelldatensatz

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09334286B2