反应详情

温度

95 °C

Methyl 2-(hydroxymethyl)-5-(trifluoromethyl)benzoate (5.00 g, 21.4 mmol) in MeOH (50 mL) was added to Pd-dppf (Heraeus) (0.312 g, 0.427 mmol) and triethylamine (5.95 ml, 42.7 mmol) in a 250 mL stainless steel pressure bottle. The mixture was pressurized with carbon monoxide (60 psi), and stirred at 95° C. for 6 hours. The mixture was filtered through Celite, and the filtrate concentrated. The residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-100% ethyl acetate in hexanes) to afford the title compound (2.5 g, 63%). MS (DCI/NH3) m/z 203 (M+H)+.

1. filtrationThe mixture was filtered through Celite
2. concentrationthe filtrate concentrated
3. customThe residue was purified by column chromatography