To a flame-dried 10-mL microwave vial with a magnetic stir bar was added 4Å MS (10 mg). The reaction vial containing molecular sieves was flame-dried for 2 minutes under vacuum and then back filled with nitrogen using a dual manifold Schlenk line. This process was repeated 3 times. After the reaction vessel had cooled to room temperature, enoxysilane 9-5 (30.0 mg, 0.053 mmol, 1.0 equiv) and DME (260 µL, 0.2 M) was added. To the stirred reaction mixture was added iodomethane (7 µL, 0.106 mmol, 2.0 equiv). The reaction vessel as then transferred to a ⎯40 °C dry-ice acetonitrile bath, and allowed to stir for 5 minutes. Following this, tetramethylammonium fluoride (7.4 mg, 0.075 mmol, 1.5 equiv) was added, which resulted in a red reaction mixture. After stirring at ⎯40 °C for 30 minutes, the reaction vessel was removed from the dry-ice acetonitrile bath and allowed to gradually warm to room temperature.