Water → HCID 86728491, compound

Participants

Reaction Steps

Under a nitrogen atmosphere, the oily product of step 3 (2.70 g) was dissolved in ethyl acetate (5.47 mL), resorcinol (1.32 g, 12.0 mmol) and methanesulfonic acid (8.20 mL, 126 mmol) were added while stirring at room temperature, and after warming to 50° C., the mixture was stirred for 4 hours. The reaction mixture was cooled to room temperature and allowed to stand for 16 hours, water (2.7 mL) was then added, and the mixture was stirred at 80° C. for 7 hours. The reaction mixture was again cooled to room temperature and allowed to stand for 16 hours, and after the mixture was warmed to 70° C., seed crystals (27.4 mg) were added. Water (5.5 mL) was then added, the mixture was stirred for 1 hour, ethanol (13.7 mL) was further added, and the mixture was stirred for 30 minutes. It was then cooled to 25° C., ethanol (38.2 mL) was added, and the mixture was stirred for 30 minutes. The precipitated crystals were collected by filtration, washed twice with ethanol (16.4 mL), and dried under reduced pressure to obtain the title compound (2.20 g).

Provenance & Evidence