1. Procedure Methyl 2-(2-acetylphenyl)acetate. An oven-dried (Note 1) 500-mL, three-necked, round-bottomed flask is equipped with a magnetic stir bar, and cesium fluoride (19.7 g, 130 mmol, 2.5 equiv) (Note 2) is added. The flask is fitted with a reflux condenser in the middle neck, an adaptor equipped with a thermometer in one of the side necks, and a septum in the other side neck. The condenser is equipped with a vacuum adaptor connected to a Schlenk line (nitrogen/vacuum manifold). The connected glassware is evacuated under high vacuum (0.025 mmHg) and carefully back-filled with nitrogen. This procedure is repeated twice to secure an oxygen-free atmosphere in the flask. Dry MeCN (260 mL) (Note 3) is added to the flask via a syringe through the septum. While stirring the reaction mixture, methyl acetoacetate (5.60 mL, 6.01 g, 51.8 mmol, 1.00 equiv) (Note 4) and 2- (trimethylsilyl)phenyl trifluoromethanesulfonate (15.7 mL, 19.3 g, 64.7 mmol, 1.25 equiv) (Note 5) are added through the septum via syringes. The flask is submerged in an oil bath (100 °C) and the reaction mixture is heated to reflux (internal temperature: 78-81 °C, reached after 15 min). The mixture is stirred at reflux temperature for 40 min (Note 6). Initially, the reaction mixture is a white opaque suspension, but during heating it changes color to yellow and upon reflux the color changes to orange. As the reaction progresses the opaque solution becomes transparent and the color changes back to yellow. Throughout the entire time a white precipitate is present in the flask. The reaction flask is removed from the oil bath and allowed to cool to ambient temperature (23 °C) over the course of 1 h. The flask is