Iodoethane → HCID 71492439, Verbindung

To a solution of 4-(((1S,2S)-1-hydroxy-2,3-dihydro-1H,1′H-[2,2′-biinden]-2-yl)methyl)benzoic acid (100 mg, 0.26 mmol) and K2CO3 (72 mg, 0.52 mmol) in DMF (2.5 mL), was added EtI (81 mg, 0.52 mmol) and then stirred at room temperature for 4 h. The reaction mixture was diluted with 1.5 N HCl (50 mL) and extracted with ethyl acetate (3×25 mL). The organic layer was washed with 10% aq. NaHCO3 (25 mL), brine (25 mL), dried over anhydrous Na2SO4 and evaporated under reduced pressure. The residue was purified by CombiFlash using 20% ethyl acetate in chloroform as an eluent to yield 55 mg (50%) of the title compound as an off white solid.

1. extractionextracted with ethyl acetate (3×25 mL)
2. washThe organic layer was washed with 10% aq. NaHCO3 (25 mL), brine (25 mL)
3. dry with materialdried over anhydrous Na2SO4
4. customevaporated under reduced pressure
5. customThe residue was purified by CombiFlash

ORD-Eintrag

ord-bc4fce5e228d4d5194cb7aa026c7197f

Quelldatensatz

uspto-grants-2016_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09260376B2