Methyl iodide → HCID 70389259, compound

Participants

Reaction Conditions

Reaction Steps

3.8 g (10 millimoles) of the benzyl alcohol derivative from Example 27, dissolved in 10 ml of dry dimethylformamide, were added dropwise to a suspension of 0.3 g (11 millimoles) of sodium hydride in 15 ml of dry dimethylformamide. The mixture was stirred until evolution of hydrogen had ended (after about 1 hour), and 1.56 g (11 millimoles) of iodomethane were then added dropwise while cooling with ice. The mixture was then heated at 60° C. for 5 hours. On the next day, water was added dropwise, and the precipitated solid was filtered off under suction, and dissolved in methanol at elevated temperature. When the solution was cooled to room temperature, 2 phases formed. The upper (methanol) phase was heated once again and then placed in a refrigerator. The precipitated crystals were filtered off under suction and dried. 2.1 g of the title compound of melting point 66°-68° C. were obtained in this manner.

Provenance & Evidence