反应详情

Trimethylsilyldiazomethane (15.71 ml, 31.4 mmol) was slowly added into a solution of (e)-4-(4-chlorophenyl)cyclohexanecarboxylic acid (3 g, 12.57 mmol) in MeOH (75 mL) at room temperature. LCMS indicated complete conversion in 1 hr. Added a few drops of TFA to quench the reaction. Volatiles were removed under reduced pressure. The resulting pot residue was purified by flash chromatography (SiO2, Biotage 65i cartridge). The column was eluted by an EtOAc/hexanes mixture (0% to 20%). Related fractions were pooled and evaporated to afford a white solid as the titled compound. LCMS calc.=252.09. found=253.20 (M+H)+.

1. customin 1 hr
2. customto quench
3. customthe reaction
4. customVolatiles were removed under reduced pressure
5. customThe resulting pot residue was purified by flash chromatography (SiO2, Biotage 65i cartridge)
6. washThe column was eluted by an EtOAc/hexanes mixture (0% to 20%)
7. customevaporated