反应详情

温度

40 °C

Dissolve 2′,4′-difluoro-biphenyl-4-carboxylic acid methyl ester (0.426 g, 1.716 mmol) in THP (5 mL) and add a solution of NaOH (0.164 g, 4.12 mmol) in water (5.0 mL). Stir the mixture for 3 d at 40° C. Concentrate in vacuo to remove THF, add 1.0M HCl until pH 2, adsorb the mixture onto silica gel, and subject the mixture to flash column chromatography (40 g column, eluting with 50% ethyl acetate/n-hexane to 100% ethyl acetate) to yield the desired-product (0.373 g, 93%). mass spectrum (m/e): 233.3 (M−1).

1. concentrationConcentrate in vacuo
2. customto remove THF
3. additionadd 1.0M HCl until pH 2, adsorb the mixture onto silica gel
4. washto flash column chromatography (40 g column, eluting with 50% ethyl acetate/n-hexane to 100% ethyl acetate)