Methanol → HCID 136082432, compound

Participants

Reaction Conditions

Reaction Steps

In an argon atmosphere, 2.3 g (6.2 millimoles) of Compound 11 obtained in Example 11 was dissolved in 100 ml of methylene chloride. The solution was cooled to 0° C. Slowly 1.8 ml (18.7 millimoles) of boron tribromide was added to the solution, and the mixture was stirred at room temperature for 7 hours. The reaction mixture was cooled to 0° C., and then 30 ml of methanol was added. The mixture was stirred at room temperature for 30 minutes. 3/4 volume of the solvent was evaporated under reduced pressure. 18 ml of 3N hydrochloric acid was added. The precipitate was collected by filtration, and recrystallized from DMF-water to obtain 2.1 g (yield: 96.3%) of Compound 14.

Provenance & Evidence