2-(3-Cyano-4-fluorophenyl)acetic acid → HCID 45925946、化合物

関与物質

反応手順

2-(3-Cyano-4-fluorophenyl)acetic acid (14.3 g, 79.8 mmol) was diluted with THF (150 mL) followed by the addition of tert-butyl N,N′-diispropylcarbamimidate (48.0 g, 239 mmol). After stirring for 12 hours, the reaction was filtered and the filtrate was concentrated. The residue was taken up in ethyl acetate 100 mL and washed with 1N HCl saturated bicarbonate water and brine. The organic layer was dried over MgSO4, filtered and concentrated. Additional precipitate was removed by filtration. The remaining residue was purified on a Biotage 40M column eluting over silica gel with hexanes:ethyl acetate (9:1) to yield tert-butyl 2-(3-cyano-4-fluorophenyl)acetate (10.0 g, 53.3% yield) as a clear oil that later solidified to a white solid.

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