This sodium hydroxide solution was then added slowly while stirring to the round bottom flask with 2. The combined solutions were allowed to stir for 30 minutes at room temperature. After 30 minutes the solution was placed in an ice water bath (0°C) for 5 minutes (note: some solid may fall out of solution). To this stirring mixture in the ice bath was added iodomethane (3.57 mL, 57.3 mmol, 1.2 eq.). The mixture was stirred rapidly to ensure distribution of iodomethane and allowed to stir overnight inside the ice water bath as it slowly warmed to room temperature. After 16 hours the suspension was immediately filtered, washed with ice water and allowed to dry for 15 minutes on filter paper before transfer to hi-vac, yielding a white powder 3 was taken forward without further purification (7.48 g, 44.0 mmol, 92%). H NMR (500 MHz, DMSO-d6) δ 12.50 (s, 1H),