Potassium Hydroxide → HCID 57567904, compound

Participants

Reaction Conditions

Reaction Steps

Under a nitrogen atmosphere, Intermediate Compound 1 (6 g, 13.4 mmol) was dissolved in 100 ml of dioxane. An aqueous solution prepared by dissolving 0.75 g (13.4 mmol) of potassium hydroxide in 5 ml of distilled water was added to the solution, and 2.56 g (16.1 mmol) of bromine were dropped to the mixture. After the resultant had been stirred on an oil bath heated to 40° C. for 30 minutes, 9.7 g (3.08 mmol) of a 5% sodium thiosulfate solution were added to the resultant, and the whole was stirred at 20° C. for an additional 2 hours. After having been filtrated, the resultant was washed with methanol and recrystallized from toluene (twice). The resultant was dried in a vacuum under heat, whereby 3.6 g of Intermediate Compound 2 were obtained.

Provenance & Evidence